Ethyl 4-piperidinecarboxylate → HCID 3422241、化合物

HRID 2381179ノート

反応式

HRID 2381179 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 3422241HCID 3422241、化合物収率 103.4%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c34ee9435c4f4c02b0366ffa1a8b94f0
出典データセット
uspto-grants-2012_09
特許番号
US08258158B2

反応ノート

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