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

HRID 1460475ノート

反応式

HRID 1460475 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-d280254be5ce4e318aa1adc0710c1cc8
出典データセット
uspto-grants-1991_12
特許番号
US05071844

反応ノート

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