Phenazepam → HCID 136353534、化合物

HRID 1076393ノート

反応式

HRID 1076393 の反応式
[Br: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.[O:21]1[CH2:26][CH2:25][N:24]([CH:27](OCC)OCC)[CH2:23][CH2:22]1>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[C:9](=[CH:27][N:24]3[CH2:25][CH2:26][O:21][CH2:22][CH2:23]3)[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

3

反応物 2

HCID 40113PhenazepamHCID 133024324-(Diethoxymethyl)morpholine

生成物 1

HCID 136353534HCID 136353534、化合物

反応条件

温度
140 °C

実験手順

A mixture consisting of 5 gm of 7-bromo-5-(2'-chloro-phenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one and 17 ml of morpholino-diethoxy-methane was heated for 90 minutes at 140°C, while stirring, and the reaction mixture was then allowed to cool. The cool product was admixed with 150 ml of petroleum ether (b.p. 60°-80°C), the mixture was briefly brought to the boiling point, allowed to cool, and the crystalline substance which had separated out was collected by vacuum filtration and recrystallized from isopropanol, yielding the compound named in the heading, which decomposed slowly between 156° and 185°C.

後処理

  1. temperatureto cool
  2. temperatureto cool
  3. customthe crystalline substance which had separated out
  4. filtrationwas collected by vacuum filtration
  5. customrecrystallized from isopropanol
  6. customyielding the compound
  7. customdecomposed slowly between 156° and 185°C.

出典と根拠

ORDレコード
ord-de986cc630c8429b80b20b08e0474375
出典データセット
uspto-grants-1976_05
特許番号
US03956492

反応ノート

読み込み中…