Piperidine → 1-[4-(1-Piperidinylsulfonyl)phenyl]ethanone

HRID 507527노트

반응식

HRID 507527 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[NH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.C(N(CC)CC)C>O1CCCC1.[Cl-].[Na+].O>[N:14]1([S:10]([C:7]2[CH:8]=[CH:9][C:4]([C:1](=[O:3])[CH3:2])=[CH:5][CH:6]=2)(=[O:12])=[O:11])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

참가 물질

6

반응물 3

HCID 8082PiperidineHCID 8471TriethylamineHCID 2664184-Acetylbenzenesulfonyl chloride

생성물 1

HCID 7503641-[4-(1-Piperidinylsulfonyl)phenyl]ethanone수율 94%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 57417360Sodium chloride; water용매

실험 절차

A mixture of 4-acetylbenzene-1-sulfonyl chloride (2 g, 9.2 mmol), piperidine (0.85 g, 10.0 mmol) and triethylamine (1.9 g, 18.4 mmol) in tetrahydrofuran (60 mL) was stirred at rt overnight. Brine (100 mL) was added and the mixture was extracted with ethyl acetate (3×100 mL). The combined organic layer was washed with brine (100 mL), dried over anhydrous sodium sulfate and filtered. Removal of solvent in vacuo gave the title compound as a white solid (2.3 g, 94%). MS (M+H)+ 268.

후처리

  1. extractionthe mixture was extracted with ethyl acetate (3×100 mL)
  2. washThe combined organic layer was washed with brine (100 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customRemoval of solvent in vacuo

출처 및 근거

ORD 기록
ord-c564f21aa14b4ac3831f7dfe5253d484
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786132B2

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