Iem 2115 → Trans-1-ethyl-4-[(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)amino]-3-pyrrolidinol (Z)-Butenedioate

HRID 126923ノート

反応式

HRID 126923 の反応式
[NH2:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][CH2:5][C:4]2[CH:13]=[CH:14][CH:15]=[CH:16][C:3]1=2.[CH2:17]([N:19]1[CH2:23][CH:22]2[O:24][CH:21]2[CH2:20]1)[CH3:18].[C:25]([O-:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([O-:30])=[O:29]>Cl>[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29].[CH2:17]([N:19]1[CH2:23][C@@H:22]([NH:1][CH:2]2[C:3]3[CH:16]=[CH:15][CH:14]=[CH:13][C:4]=3[CH2:5][CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]2=3)[C@H:21]([OH:24])[CH2:20]1)[CH3:18]

参加物

5

反応物 3

HCID 81481Iem 2115HCID 5288227Maleate(2-)HCID 13320194N-ethyl-3,4-epoxypyrrolidine

生成物 1

HCID 86737534Trans-1-ethyl-4-[(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)amino]-3-pyrrolidinol (Z)-Butenedioate

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid触媒

反応条件

温度
140 °C

実験手順

A mixture of 7.5 g (0.036 mole) of 5-amino-10,11-dihydro-5H-dibenzo[a,d]cycloheptene, 4.1 g (0.036 mole) of n-ethyl-3,4-epoxypyrrolidine and 2 drops concentrated hydrochloric acid was heated at 140° C. under a nitrogen atmosphere overnight. The residue was converted to the maleate. The salt was recrystallized twice from isopropyl alcohol, converted to the base, reconverted to the maleate, and recrystallized from isopropyl alcohol to yield 1.4 g. (7%) of white solid, m.p. 132°-135° C.

後処理

  1. customThe salt was recrystallized twice from isopropyl alcohol
  2. customrecrystallized from isopropyl alcohol
  3. customto yield 1.4 g

出典と根拠

ORDレコード
ord-c7a9b1408ab8447a96ede91574336901
出典データセット
uspto-grants-1981_03
特許番号
US04254135

反応ノート

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