Ethanol → 7-Chloro-5-(2'-chloro-phenyl)-1,3-dihydro-3-(dimethylaminomethylene)-2H-1,4-benzodiazepin-2-one

HRID 1076389ノート

反応式

HRID 1076389 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1.C(O)C.C(O[CH:27](OCC)[N:28]([CH3:30])[CH3:29])C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[C:9](=[CH:27][N:28]([CH3:30])[CH3:29])[N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1

参加物

4

反応物 3

HCID 702EthanolHCID 17925DelorazepamHCID 70913Dimethylformamide diethylacetal

生成物 1

HCID 1363535337-Chloro-5-(2'-chloro-phenyl)-1,3-dihydro-3-(dimethylaminomethylene)-2H-1,4-benzodiazepin-2-one

反応条件

温度
130 °C

実験手順

A suspension of 50 gm of 7-chloro-5-(2'-chlorophenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one in 100 ml of N,N-dimethyl-formamide diethylacetal was heated to 130°C in a vessel equipped with a descending condenser, whereby a clear solution was formed after a short time. The temperature of the reaction solution was maintained at 130°C for 40 minutes, during which time the ethanol formed by the reaction slowly distilled over. Thereafter, the reaction solution was allowed to cool, and the red precipitate was collected by vacuum filtration, washed with petroleum ether and recrystallized from methanol, whereupon it had a melting point of 239°-241°C. It was identified to be the compound of the formula ##SPC6##

後処理

  1. customequipped with a descending condenser
  2. customwhereby a clear solution was formed after a short time
  3. customformed by the reaction
  4. distillationslowly distilled over
  5. temperatureto cool
  6. filtrationthe red precipitate was collected by vacuum filtration
  7. washwashed with petroleum ether
  8. customrecrystallized from methanol, whereupon it

出典と根拠

ORDレコード
ord-7f87dbed62cc469cb7913123ec3770ae
出典データセット
uspto-grants-1976_05
特許番号
US03956492

反応ノート

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