1,3,4-Thiadiazol-2-amine → 2-{3-(2-Chloroethyl)-3-nitrosoureido}-1,3,4-thiadiazole

HRID 1156405

반응식

HRID 1156405 반응식
[NH2:1][C:2]1[S:3][CH:4]=[N:5][N:6]=1.[Cl:7][CH2:8][CH2:9][N:10]([N:16]=[O:17])[C:11](N=[N+]=[N-])=[O:12]>N1C=CC=CC=1>[Cl:7][CH2:8][CH2:9][N:10]([N:16]=[O:17])[C:11](=[O:12])[NH:1][C:2]1[S:3][CH:4]=[N:5][N:6]=1

참가 물질

4

반응물 2

HCID 199091,3,4-Thiadiazol-2-amineHCID 10654895N-(2-chloroethyl)-N-nitrosocarbamoylazide

생성물 1

HCID 130029522-{3-(2-Chloroethyl)-3-nitrosoureido}-1,3,4-thiadiazole수율 76.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Ten grams of 2-amino-1,3,4-thiadiazole was dissolved in 100 ml of pyridine, and cooled with ice. While stirring the solution, 26.5 g of N-(2-chloroethyl)-N-nitrosocarbamoyl azide was gradually added, and after the addition, the stirring was continued for 60 minutes. The reaction solution was poured into ice water, and the precipitated crystals were washed with water, dried and recrystallized from methanol, to obtain 17.8 g (Yield 75%) of 2-{3-(2-chloroethyl)-3-nitrosoureido}-1,3,4-thiadiazole. The physical properties of this compound were identical with those of the compound obtained by Example 1.

후처리

  1. temperaturecooled with ice
  2. additionwas gradually added
  3. additionafter the addition
  4. washthe precipitated crystals were washed with water
  5. customdried
  6. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-9b38d1c485114ce5ade8676781ede09e
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04335247

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