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

HRID 126923노트

반응식

HRID 126923 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid촉매

반응 조건

온도
140 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c7a9b1408ab8447a96ede91574336901
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254135

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