Maleic Acid → (S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine maleate

HRID 1460475노트

반응식

HRID 1460475 반응식
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][O:10][C:11]1[CH:39]=[CH:38][C:14]([CH2:15][CH2:16][N:17]2[CH2:21][CH2:20][CH2:19][C@H:18]2[CH2:22][N:23]2[C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=3[CH2:27][S:26][C:25]3[CH:34]=[CH:35][CH:36]=[CH:37][C:24]2=3)=[CH:13][CH:12]=1>C(OCC)(=O)C>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][O:10][C:11]1[CH:12]=[CH:13][C:14]([CH2:15][CH2:16][N:17]2[CH2:21][CH2:20][CH2:19][C@H:18]2[CH2:22][N:23]2[C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=3[CH2:27][S:26][C:25]3[CH:34]=[CH:35][CH:36]=[CH:37][C:24]2=3)=[CH:38][CH:39]=1

참가 물질

4

반응물 2

HCID 444266Maleic AcidHCID 9824029(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine

생성물 1

HCID 9937325(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine maleate수율 64%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of maleic acid (4.7 g) in ethyl acetate (200 ml) was added to a solution of (S)-5,11-dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine (see Examples 1 and 6) (17.3 g) in ethyl acetate (100 ml) and the mixture was stirred at room temperature for 16 hours. The resulting precipitate was collected, dried and recrystallised from ethyl acetate/methanol to give the title compound as colourless crystals, (14.0 g, 64%), m.p. 153°-154° C., [α]58925 -39.7° (c=0.755 in ethanol).

후처리

  1. customThe resulting precipitate was collected
  2. customdried
  3. customrecrystallised from ethyl acetate/methanol

출처 및 근거

ORD 기록
ord-d280254be5ce4e318aa1adc0710c1cc8
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05071844

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