Ethyl 4-piperidinecarboxylate → HCID 3422241, 화합물

HRID 2381179노트

반응식

HRID 2381179 반응식
[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=[O:5])[CH3:2].[N:12]1([S:18](Cl)(=[O:20])=[O:19])[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1>C(Cl)Cl.CN(C)C1C=CN=CC=1>[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([S:18]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)(=[O:20])=[O:19])[CH2:8][CH2:7]1)=[O:5])[CH3:2]

참가 물질

5

반응물 2

HCID 70770Ethyl 4-piperidinecarboxylateHCID 12798265Morpholine-4-sulfonyl chloride

생성물 1

HCID 3422241HCID 3422241, 화합물수율 103.4%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

Piperidine-4-carboxylic acid ethyl ester (0.943 g) dissolved in methylene chloride (60 ml) under an argon atmosphere was treated at RT, first with 4-dimethylaminopyridine (1.465 g) then dropwise with morpholine-4-sulfonyl chloride (1.136 g) and the reaction mixture was stirred for 12 h at RT to complete the reaction. The reaction mixture was then partitioned between methylene chloride and aqueous 1N HCL, the layers were separated and the organic layer washed with 2M aqueous KHCO3 then dried over Na2SO4. The solvent was evaporated off, to give 1-(morpholine-4-sulfonyl)-piperidine-4-carboxylic acid ethyl ester (1.9 g) as a light yellow solid which was directly used in the next step.

후처리

  1. customthe reaction
  2. customThe reaction mixture was then partitioned between methylene chloride and aqueous 1N HCL
  3. customthe layers were separated
  4. washthe organic layer washed with 2M aqueous KHCO3
  5. dry with materialthen dried over Na2SO4
  6. customThe solvent was evaporated off

출처 및 근거

ORD 기록
ord-c34ee9435c4f4c02b0366ffa1a8b94f0
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258158B2

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