Pyridine → Chloromethyl 2-(1-(tert-butoxycarbonyl)-4-piperidyl)-ethyl carbonate

HRID 852338

反応式

HRID 852338 の反応式
N1C=CC=CC=1.[C:7]([O:11][C:12]([N:14]1[CH2:19][CH2:18][CH:17]([CH2:20][CH2:21][OH:22])[CH2:16][CH2:15]1)=[O:13])([CH3:10])([CH3:9])[CH3:8].Cl[C:24]([O:26][CH2:27][Cl:28])=[O:25]>ClCCl>[C:24](=[O:25])([O:22][CH2:21][CH2:20][CH:17]1[CH2:18][CH2:19][N:14]([C:12]([O:11][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:13])[CH2:15][CH2:16]1)[O:26][CH2:27][Cl:28]

参加物

5

反応物 3

HCID 1049PyridineHCID 62754Chloromethyl chloroformateHCID 8541401-(tert-Butoxycarbonyl)-4-(2-hydroxyethyl)piperidine

生成物 1

HCID 69348251Chloromethyl 2-(1-(tert-butoxycarbonyl)-4-piperidyl)-ethyl carbonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Pyridine (3.22 ml) was added to an ice-cold solution of 2-(1-(tert-butoxycarbonyl)-4-piperidyl)-ethanol (7.6 g) in dichloromethane (33 ml) followed by chloromethyl chloroformate (3.23 ml) at such a rate that the temperature was kept below 10° C. After stirring overnight at room temperature the reaction mixture was washed twice with 0.5 M HCl followed by water and aqueous sodium bicarbonate. The organic phase was dried over magnesium sulfate, filtered and evaporated in vacuo to yield the title compound as a colourless oil.

後処理

  1. customwas kept below 10° C
  2. washwas washed twice with 0.5 M HCl
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-00a2fcaf0e5e459c942f851bfe62a8ff
出典データセット
uspto-grants-2007_08
特許番号
US07253193B2

関連ノート

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