Water → HCID 68687571、化合物

HRID 2244216ノート

反応式

HRID 2244216 の反応式
[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:6]=[CH:5][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[CH:20]=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:3][CH:2]=1.[Cl:29][C:30]([Cl:35])([Cl:34])[C:31](Cl)=[O:32].O>O1CCOCC1>[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:2]=[CH:3][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[C:20]([C:31](=[O:32])[C:30]([Cl:35])([Cl:34])[Cl:29])=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 6420Trichloroacetyl chlorideHCID 9799174HCID 9799174、化合物

生成物 1

HCID 68687571HCID 68687571、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

10-(1,1′-Biphenyl-4-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Step A (1.822 g; 0.005 mol) was dissolved in 50 mL of 1,4-dioxane to which was then added 0.946 g (0.0052 mol) of trichloroacetyl chloride. The reaction solution was heated under reflux with stirring over night, cooled to room temperature and then poured into 250 mL of water. Recrystallization of the crude material from ethanol provided a solid, m.p. 197-198° C.

後処理

  1. temperatureThe reaction solution was heated
  2. temperatureunder reflux
  3. customRecrystallization of the crude material from ethanol
  4. customprovided a solid, m.p. 197-198° C.

出典と根拠

ORDレコード
ord-e83aa627fea141a297d2ee9749e36791
出典データセット
uspto-grants-2010_03
特許番号
US07678787B2

反応ノート

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