Methanesulfonyl chloride → (+/-)-6-Methoxy-2-methyl-3-[1-(methylsulfonyl)piperidin-3-yl]-4-phenylisoquinolin-1(2H)-one

HRID 17869노트

반응식

HRID 17869 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=[O:13])[N:8]([CH3:14])[C:7]([CH:15]1[CH2:20][CH2:19][CH2:18][NH:17][CH2:16]1)=[C:6]2[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(N(CC)C(C)C)(C)C.[CH3:36][S:37](Cl)(=[O:39])=[O:38].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=[O:13])[N:8]([CH3:14])[C:7]([CH:15]1[CH2:20][CH2:19][CH2:18][N:17]([S:37]([CH3:36])(=[O:39])=[O:38])[CH2:16]1)=[C:6]2[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

참가 물질

6

반응물 4

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 11279492(+/-)-6-Methoxy-2-methyl-4-phenyl-3-piperidin-3-ylisoquinolin-1(2H)-one

생성물 1

HCID 11327779(+/-)-6-Methoxy-2-methyl-3-[1-(methylsulfonyl)piperidin-3-yl]-4-phenylisoquinolin-1(2H)-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a methylene chloride (0.100 mL) solution of (±)-6-methoxy-2-methyl-4-phenyl-3-piperidin-3-ylisoquinolin-1(2H)-one (30 mg, 0.086 mmol) and N,N-diisopropylethylamine (0.017 mL, 0.095 mmol) was added methanesulfonyl chloride (0.007 mL, 0.095 mmol). After 24 hours saturated sodium bicarbonate and additional methylene chloride were added. The layers were separated and the organic phase dried with anhydrous magnesium sulfate. Evaporation of the solvent in vacuo followed by trituration with ether-EtOAc gave a white solid which was isolated by vacuum filtration to give the titled product. ESI+MS: 427.1 [M+H]+.

후처리

  1. customThe layers were separated
  2. dry with materialthe organic phase dried with anhydrous magnesium sulfate
  3. customEvaporation of the solvent in vacuo
  4. customgave a white solid which
  5. customwas isolated by vacuum filtration

출처 및 근거

ORD 기록
ord-6c3f74d63301475dbdfd131f9419fa5c
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741322B2

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