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Pyridine → 2-t-Butoxycarbonylamino-1-chloro-1-phenylethane

HRID 256010
ノート
印刷プレビュー

反応式

HRID 256010 の反応式
N1C=CC=CC=1.CS([Cl:11])(=O)=O.[C:12]([O:16][C:17]([NH:19][CH2:20][CH:21]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)O)=[O:18])([CH3:15])([CH3:14])[CH3:13]>C(Cl)Cl>[C:12]([O:16][C:17]([NH:19][CH2:20][CH:21]([Cl:11])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:18])([CH3:15])([CH3:14])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 9816137tert-butyl N-(2-hydroxy-2-phenylethyl)carbamate

生成物 1

HCID 201649052-t-Butoxycarbonylamino-1-chloro-1-phenylethane

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3.7 ml of pyridine and 2.2 ml of methanesulfonyl chloride was added dropwise to 35 ml of a solution of 3.5 g of 2-t-butoxycarbonylamino-1-phenylethanol [prepared as described in step (a) above] in methylene chloride and the reaction mixture was allowed to stand overnight at room temperature. The reaction mixture was condensed by evaporation under reduced pressure, and the residue was dissolved in a mixture of ethyl acetate and water. The ethyl acetate layer was separated, washed with water and then washed with an aqueous solution of potassium hydrogen sulfate and with an aqueous solution of sodium bicarbonate. The resulting solution was dried over anhydrous magnesium sulfate. The solvent was then distilled off. The residue was subjected to silica gel column chromatography using a 15:85 by volume mixture of ethyl acetate and cyclohexane as the eluent, to give 0.75 g of the title compound as crystals melting at 57°-59° C.

後処理

  1. customcondensed
  2. customby evaporation under reduced pressure
  3. dissolutionthe residue was dissolved in a mixture of ethyl acetate and water
  4. customThe ethyl acetate layer was separated
  5. washwashed with water
  6. washwashed with an aqueous solution of potassium hydrogen sulfate and with an aqueous solution of sodium bicarbonate
  7. dry with materialThe resulting solution was dried over anhydrous magnesium sulfate
  8. distillationThe solvent was then distilled off
  9. additionby volume mixture of ethyl acetate and cyclohexane as the eluent

出典と根拠

ORDレコード
ord-9d104671dae6416aa1b3d071dae842f6
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04699905

反応ノート

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