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Ethyl chloroformate → ethyl N-(1-benzylpiperidin-4-yl)carbamate

HRID 1090691
ノート
印刷プレビュー

反応式

HRID 1090691 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[NH2:7][CH:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:10][CH2:9]1>N1C=CC=CC=1>[C:15]1([CH2:14][N:11]2[CH2:12][CH2:13][CH:8]([NH:7][C:2](=[O:3])[O:4][CH2:5][CH3:6])[CH2:9][CH2:10]2)[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 4158521-Benzyl-4-piperidylamine

生成物 1

HCID 12641845ethyl N-(1-benzylpiperidin-4-yl)carbamate収率 62.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Ethyl chloroformate (30 g, 0.276 mol) was added at 0° C. to 4-amino-1-phenylmethylpiperidine (50 g, 0.262 mol) in pyridine (600 mL). After the addition, the mixture was kept at room temperature overnight, and the pyridine was then evaporated. The residue was extracted with methylene chloride; and the resulting solution washed with water, dried over sodium sulfate, and the methylene chloride evaporated to dryness. The residue was dissolved in diisopropyl ether. A white product precipitated, which was isolated by filtration to yield 42.71 g (62%) of ethyl (1-phenylmethyl-4-piperidyl)-carbamate, m.p. 100° C.

後処理

  1. additionAfter the addition
  2. customthe pyridine was then evaporated
  3. extractionThe residue was extracted with methylene chloride
  4. washand the resulting solution washed with water
  5. dry with materialdried over sodium sulfate
  6. customthe methylene chloride evaporated to dryness
  7. dissolutionThe residue was dissolved in diisopropyl ether
  8. customA white product precipitated
  9. customwhich was isolated by filtration

出典と根拠

ORDレコード
ord-0fe390e75e8e454c8ded6931d2c958fc
出典データセット
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05082847

反応ノート

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