Triethylamine → tert-Butyl 4-(2-((methanesulfonyl)oxy)ethyl)piperidine-1-carboxylate

HRID 54544ノート

反応式

HRID 54544 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][CH2:7][CH2:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]1.C(N(CC)CC)C>C(Cl)Cl>[C:18]([O:17][C:15]([N:12]1[CH2:11][CH2:10][CH:9]([CH2:8][CH2:7][O:6][S:2]([CH3:1])(=[O:4])=[O:3])[CH2:14][CH2:13]1)=[O:16])([CH3:21])([CH3:20])[CH3:19]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 8541401-(tert-Butoxycarbonyl)-4-(2-hydroxyethyl)piperidine

生成物 1

HCID 15229596tert-Butyl 4-(2-((methanesulfonyl)oxy)ethyl)piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of methanesulfonyl chloride (0.51 ml) in methylene chloride (5 ml) was added dropwise to a mixture of 4-(2-hydroxyethyl)-1-tert-butoxycarbonylpiperidine (1.43 g) and triethylamine (0.91 ml) at 5° C. After stirring at ambient temperature for 1 hour, the mixture was poured into ice water and extracted with ethyl acetate. The extract was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo to give 1-tert-butoxycarbonyl-4-(2-mesyloxyethyl)piperidine (1.37 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-5cfeb3dd818c45089f6ebdb5dc7bffac
出典データセット
uspto-grants-1997_04
特許番号
US05622976

反応ノート

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