Hydrazine hydrate (1:1) → HCID 67713383、化合物

HRID 1378257ノート

反応式

HRID 1378257 の反応式
O.[NH2:2][NH2:3].[CH3:4][N:5]1[C:11](=[O:12])[C:10]2[S:13][CH:14]=[CH:15][C:9]=2[N:8]2[CH:16]=[N:17][C:18]([C:19]([O:21]CC)=O)=[C:7]2[CH2:6]1>C(O)C>[CH3:4][N:5]1[C:11](=[O:12])[C:10]2[S:13][CH:14]=[CH:15][C:9]=2[N:8]2[CH:16]=[N:17][C:18]([C:19]([NH:2][NH2:3])=[O:21])=[C:7]2[CH2:6]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 22914412HCID 22914412、化合物

生成物 1

HCID 67713383HCID 67713383、化合物収率 97%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

13 ml of hydrazine hydrate were added to a suspension of 7.0 g (24 mmol) of ethyl 5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a]thieno[2,3-f][1,4]diazepine-3-carboxylate in 70 ml of ethanol and the mixture was heated at reflux for 3 hours. After cooling to 0° the crystals obtained were filtered off and there were obtained 6.5 g (97%) of 5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a]thieno[2,3-f][1,4]diazepine-3-carboxylic acid hydrazide as colourless needles of m.p. >260°.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 3 hours
  3. temperatureAfter cooling to 0° the crystals
  4. customobtained
  5. filtrationwere filtered off

出典と根拠

ORDレコード
ord-d207d70899d44470abe7f2a5b36984aa
出典データセット
uspto-grants-1997_09
特許番号
US05665718

反応ノート

読み込み中…