Thiourea → HCID 21995603、化合物

HRID 1977815ノート

反応式

HRID 1977815 の反応式
Br[CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][C:6]([N+:11]([O-:13])=[O:12])=[CH:7][CH:8]=2)[C:3]1=[O:14].[NH2:15][C:16]([NH2:18])=[S:17]>CC(C)=O>[NH2:18][C:16]1[S:17][CH:2]2[CH2:10][C:9]3[CH:8]=[CH:7][C:6]([N+:11]([O-:13])=[O:12])=[CH:5][C:4]=3[C:3]2([OH:14])[N:15]=1

参加物

4

反応物 2

HCID 2723790ThioureaHCID 110650202-Bromo-6-nitro-1-indanone

生成物 1

HCID 21995603HCID 21995603、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

1.28 g (5 mmol) of 2-bromo-6-nitroindan-1-one are dissolved in 30 ml of acetone and, while stirring, 530 mg of thiourea in 10 ml of acetone are added. The solution is initially clear but, after a few minutes, the hydrobromide of 2-amino-5-nitro-8,8a-dihydroindeno[1,2-d]thiazol-3a-ol crystallizes out. It is stirred at room temperature for 1 h, filtered off with suction and washed with a little acetone. The air-dried hydrobromide is dissolved in about 10 ml of methanol and, after addition of 0.7 ml of triethylamine, stirred for 15 min. Then 50 ml of water are added, and the mixture is stirred at room temperature for 1 h. The crystals which have formed are filtered off with suction and washed with a little cold water. 2-Amino-5-nitro-8,8a-dihydroindeno[1,2-d]thiazol-3a-ol is obtained with a melting point above 250° C.

後処理

  1. waitThe solution is initially clear but, after a few minutes
  2. customthe hydrobromide of 2-amino-5-nitro-8,8a-dihydroindeno[1,2-d]thiazol-3a-ol crystallizes out
  3. stirringIt is stirred at room temperature for 1 h
  4. filtrationfiltered off with suction
  5. washwashed with a little acetone
  6. dissolutionThe air-dried hydrobromide is dissolved in about 10 ml of methanol
  7. additionafter addition of 0.7 ml of triethylamine
  8. stirringstirred for 15 min
  9. additionThen 50 ml of water are added
  10. stirringthe mixture is stirred at room temperature for 1 h
  11. customThe crystals which have formed
  12. filtrationare filtered off with suction
  13. washwashed with a little cold water

出典と根拠

ORDレコード
ord-7155f5b2e2e74916a814f0a8d37a9c27
出典データセット
uspto-grants-2001_05
特許番号
US06235763B1

反応ノート

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