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Ethyl chloroformate → Ethyl 4-acetamidopiperidine-1-carboxylate

HRID 1017548
ノート
印刷プレビュー

反応式

HRID 1017548 の反応式
[C:1]([NH:4][CH:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)(=[O:3])[CH3:2].C(=O)(O)[O-].[Na+].Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18]>O.C(OCC)(=O)C>[C:1]([NH:4][CH:5]1[CH2:10][CH2:9][N:8]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:7][CH2:6]1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10928Ethyl chloroformateHCID 516892Sodium BicarbonateHCID 14451564-Acetamidopiperidine

生成物 1

HCID 18403966Ethyl 4-acetamidopiperidine-1-carboxylate収率 103.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4-acetamidopiperidine (20.7 g), sodium bicarbonate (10.6 g) and water (300 ml) was cooled to 0° C., and 17.7 g of ethyl chloroformate was added dropwise, with stirring. Upon completion of the addition, the reaction mixture was allowed to warm to ambient temperature and was diluted with water and ethyl acetate. The layers were separated, and the organic layer was washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated to give 32.2 g (100%) of product.

後処理

  1. additionUpon completion of the addition
  2. customThe layers were separated
  3. washthe organic layer was washed with saturated sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customThe filtrate was evaporated

出典と根拠

ORDレコード
ord-61fbb833083e4e3aa2a632c22d4d75b2
出典データセット
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06479501B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート