Hexamethylenetetramine → 2-Oxoquazepam

HRID 262944

反応式

HRID 262944 の反応式
Br[CH2:2][C:3]([N:5]([C:11]1[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:12]=1[C:13]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[F:21])=O)[CH2:6][C:7]([F:10])([F:9])[F:8])=[O:4].C1N2CN3CN(C2)C[N:28]1C3.[Br-].[NH4+]>O>[Cl:26][C:23]1[CH:24]=[CH:25][C:11]2[N:5]([CH2:6][C:7]([F:10])([F:9])[F:8])[C:3](=[O:4])[CH2:2][N:28]=[C:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[F:21])[C:12]=2[CH:22]=1

参加物

5

反応物 3

HCID 4101HexamethylenetetramineHCID 25514Ammonium BromideHCID 21317109HCID 21317109、化合物

生成物 1

HCID 932502-Oxoquazepam

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Reflux 1.13 g. (0.0025 moles) of 2-[2-bromo-N-(2,2,2-trifluoroethyl)-acetamido]-5-chloro-2'-fluorobenzophenone, 1.4 g. (0.01 mole) of hexamethylenetetramine, and 0.98 g. (0.01 moles) of ammonium bromide together for 43/4 hours. Pour the reaction mixture into water and extract with dichloromethane. Dry the dichloromethane solution over anhydrous sodium sulfate, filter and evaporate. After recrystallization, the so-obtained 7-chloro-1,3-dihydro-1-(2,2,2-trifluoroethyl)-5-(2'fluorophenyl)-2H-1,4-benzodiazepin-2-one melts at 123°-125° C. Thin layer chromatography shows the product to be pure single spot material.

後処理

  1. temperatureReflux 1.13 g
  2. custom4 hours
  3. extractionextract with dichloromethane
  4. dry with materialDry the dichloromethane solution over anhydrous sodium sulfate
  5. filtrationfilter
  6. customevaporate
  7. customAfter recrystallization

出典と根拠

ORDレコード
ord-c14b13ac586c4799895637567272b71e
出典データセット
uspto-grants-1979_05
特許番号
US04155904

関連ノート

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