Hydrogen Sulfide → 2,4-Diamino-5-pyrimidinecarbothioamide

HRID 2285590

반응식

HRID 2285590 반응식
[SH2:1].[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([C:10]#[N:11])=[CH:5][N:4]=1.C(N(CC)CC)C.N1C=CC=CC=1>CS(C)=O.O>[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([C:10](=[S:1])[NH2:11])=[CH:5][N:4]=1

참가 물질

7

반응물 4

HCID 402Hydrogen SulfideHCID 1049PyridineHCID 8471TriethylamineHCID 2821152,4-Diaminopyrimidine-5-carbonitrile

생성물 1

HCID 128311672,4-Diamino-5-pyrimidinecarbothioamide

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

Hydrogen sulfide is passed into a mixture of 2,4-diamino-5-pyrimidine carbonitrile (10.000 g., 0.0740 mole), triethylamine (10.3 ml., 0.0740 mole) and pyridine (6.0 ml., 0.074 mole) in dimethyl sulfoxide (100 ml.) for one-half hour. After storage at room temperature overnight, the brown solution is poured into water (500 ml.) with stirring. The product separates as a yellow crystalline solid which is collected by filtration, washed with water, dried at 56° C./0.1 mm. The yield of crude product melting at greater than 325° C. (uncorr.) is 12.020 g. (96.0%). Recrystallization of this material from 2-methoxyethanol affords the title compound as tan crystals melting above 350° C. (uncorr.) after drying at 110° C. at 0.1 mm.

후처리

  1. filtrationis collected by filtration
  2. washwashed with water
  3. customdried at 56° C./0.1 mm
  4. customRecrystallization of this material from 2-methoxyethanol

출처 및 근거

ORD 기록
ord-89fc12e9952040d99ae28d69e8624f5c
출처 데이터셋
uspto-grants-1982_04
특허 번호
US04323681

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