SUMMARYA safe procedure for the conversion of barium carbonate-I4C to potassium cyanide-I4C on a 6-7 mmol scale in 90-98% yield was developed. Barium carbonate-14C was heated with excess potassium azide in a matrix of sand without added potassium metal, allowing safe, rapid and convenient recovery of the cyanide.
A series of analogs of thyroliberin (TRH) ([L‐3Pro3]‐TRH, [D‐3Pro3]‐TRH, [L‐3‐MeHis2, L‐3Pro3]‐TRH) in which proline was replaced by L‐ or D‐3, 4‐dehydroproline was synthesized. The analogs exhibited approximately the same biological activity as the corresponding proline‐containing peptides. These analogs and others in which 3, 4‐dehydroproline is present at the NH2‐terminal, COOH‐terminal or internal positions in the peptide were successfully reduced with deuterium or tritium to provide the 3, 42‐H2‐proline or 3, 43‐H2‐proline analogs, respectively, with near theoretical values of substitution. A novel procedure for the chemical resolution of DL‐3, 4‐dehydroproline is also described.
A new type of differential manometer is described, which utilizes a flexible brass bellows and a Statham Strain Gage. The manometer may be made sensitive to a differential pressure of 10*"8 mm. of mercury. This instrument was used as a null point indicator in comparing the temperatures of equal vapor pressure of potassium chloride solutions and pure water. The results indicate that high precision is possible, with temperature measurement and control the limiting factors.
SUMMARYBromination of 4'-phthalimidomethyltrioxsalen (3) provided the 3-monobromo derivative (4) which on hydrogenolysis with either deuterium or tritium provided the corresponding labelled derivatives Removal of the phthalimide moiety from 6 produced the title compound (2) having specific activity of 7.46 Ci/mmole. and 5.
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