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

HRID 1460476노트

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HRID 1460476 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-71a82233e1a1419aa062770e9915adcd
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05071844

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