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

HRID 1460476ノート

反応式

HRID 1460476 の反応式
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:36]=[CH:35][C:11]([CH2:12][CH2:13][N:14]2[CH2:18][CH2:17][CH2:16][C@H:15]2[CH2:19][N:20]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[CH2:24][S:23][C:22]3[CH:31]=[CH:32][CH:33]=[CH:34][C:21]2=3)=[CH:10][CH:9]=1>ClCCl>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([CH2:12][CH2:13][N:14]2[CH2:18][CH2:17][CH2:16][C@H:15]2[CH2:19][N:20]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[CH2:24][S:23][C:22]3[CH:31]=[CH:32][CH:33]=[CH:34][C:21]2=3)=[CH:35][CH:36]=1

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 9824029(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine

生成物 1

HCID 88452751(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine methanesulphonate収率 70.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methanesulphonic acid (39 mg) 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) (175 mg) in dichloromethane (5 ml) and the mixture was stirred at room temperature for 16 hours and evaporated under reduced pressure. The residue was crystallised from ethyl acetate/diisopropyl ether to give the title compound as colourless crystals, (150 mg, 31%), m.p. 118°-122° C., [α]58925 -36.9° (c=0.59 in ethanol).

後処理

  1. customevaporated under reduced pressure
  2. customThe residue was crystallised from ethyl acetate/diisopropyl ether

出典と根拠

ORDレコード
ord-71a82233e1a1419aa062770e9915adcd
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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