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

HRID 1156405

反応式

HRID 1156405 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9b38d1c485114ce5ade8676781ede09e
出典データセット
uspto-grants-1982_06
特許番号
US04335247

関連ノート

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