Hydrazine hydrate (1:1) → 2-[(1-benzyl-1H-1,3-benzodiazol-2-yl)sulfanyl]acetohydrazide

HRID 507263

反応式

HRID 507263 の反応式
[CH2:1]([N:8]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]=[C:9]1[S:17][CH2:18][C:19]([O:21]CC)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:25][NH2:26]>C(O)C>[CH2:1]([N:8]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]=[C:9]1[S:17][CH2:18][C:19]([NH:25][NH2:26])=[O:21])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 975431ethyl [(1-benzyl-1H-benzimidazol-2-yl)sulfanyl]acetate

生成物 1

HCID 8769682-[(1-benzyl-1H-1,3-benzodiazol-2-yl)sulfanyl]acetohydrazide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of ethyl 2-(1-benzyl-1H-benzo[d]imidazol-2-ylthio)acetate 4b (200 mg, 0.61 mmol, 1.0 eq.) in ethanol (5 mL), was added hydrazine monohydrate (61 mg, 1.23 mmol, 2.0 eq.), and the reaction mixture was heated to reflux and stirred at that temperature for 16 hours. The reaction mixture was cooled to room temperature and concentrated in vacuo. The mixture was dissolved in ethyl acetate (20 mL) and washed with water (20 mL) and brine (20 mL). The organic layer was dried over magnesium sulfate and concentrated in vacuo giving 4c as a pale yellow solid which was used without further purification (200 mg, 100%).

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux
  3. concentrationconcentrated in vacuo
  4. dissolutionThe mixture was dissolved in ethyl acetate (20 mL)
  5. washwashed with water (20 mL) and brine (20 mL)
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-19c866b97c1447c48c70ba5ff7ddf59d
出典データセット
uspto-grants-2010_08
特許番号
US07786139B2

関連ノート

読み込み中…