Ethanol → HCID 12874074、化合物

HRID 461558ノート

反応式

HRID 461558 の反応式
Cl.[CH3:2][N:3]([CH3:11])[CH:4]1[CH2:9][CH2:8][C:7](=O)[CH2:6][CH2:5]1.Cl.[CH2:13]([O:20][C:21]1[CH:22]=[C:23]([NH:27]N)[CH:24]=[CH:25][CH:26]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(O)C>O>[CH3:2][N:3]([CH3:11])[CH:4]1[CH2:9][C:8]2[C:24]3[C:23](=[CH:22][C:21]([O:20][CH2:13][C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=4)=[CH:26][CH:25]=3)[NH:27][C:7]=2[CH2:6][CH2:5]1

参加物

5

反応物 3

HCID 702EthanolHCID 127174484-(Dimethylamino)cyclohexan-1-one--hydrogen chloride (1/1)HCID 12891839(3-(Benzyloxy)phenyl)hydrazine hydrochloride

生成物 1

HCID 12874074HCID 12874074、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 15.8 g. of 4-dimethylaminocyclohexanone hydrochloride and 20.3 g. of 3-benzyloxyphenylhydrazine hydrochloride (m.p. 165°-168° C.) in 225 ml. of absolute ethyl alcohol was heated under reflux for three hours, cooled to room temperature, and diluted with 50 ml. of water. After standing for three hours the resulting crystals were collected by filtration and washed with ethyl alcohol to give, after recrystallization from ethyl alcohol, 6.1 g. of 3-(dimethylamino)-7-(benzyloxy)-1,2,3,4-tetrahydrocarbazole hydrochloride, m.p. 237°-239° C.

後処理

  1. temperatureunder reflux for three hours
  2. additiondiluted with 50 ml
  3. filtrationthe resulting crystals were collected by filtration
  4. washwashed with ethyl alcohol
  5. customto give
  6. customafter recrystallization from ethyl alcohol, 6.1 g

出典と根拠

ORDレコード
ord-dc411932b4a94c0084520834d420f485
出典データセット
uspto-grants-1977_12
特許番号
US04062864

反応ノート

読み込み中…