Water → (S)-(1,2,3,4-tetrahydro-naphthalen-1-yl)carbamic acid ethyl ester

HRID 606292

反応式

HRID 606292 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[C@@H:7]1([NH2:17])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH2:10][CH2:9][CH2:8]1.C([O-])([O-])=O.[K+].[K+].O>CC#N>[CH2:5]([O:4][C:2](=[O:3])[NH:17][C@@H:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH2:10][CH2:9][CH2:8]1)[CH3:6]

参加物

6

反応物 4

HCID 962WaterHCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 70580741-Aminotetralin, (S)-

生成物 1

HCID 7768470(S)-(1,2,3,4-tetrahydro-naphthalen-1-yl)carbamic acid ethyl ester

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Ethyl chloroformate (7.74 g, 71.3 mmol) is added dropwise to a mixture of (S)-1,2,3,4-tetrahydro-naphthalen-1-ylamine (10.0 g, 67.9 mmol) and K2CO3 (18.8 g, 136 mmol) in CH3CN (100 mL). The resulting mixture is stirred at room temperature overnight. Water (100 mL) is added and the mixture is extracted with ether (2×100 mL). The combined extract is washed with 1 N HCl (2×10 mL), water, dried (Na2SO4), and concentrated in vacuo to give (S)-(1,2,3,4-tetrahydro-naphthalen-1-yl)-carbamic acid ethyl ester as a solid.

後処理

  1. extractionthe mixture is extracted with ether (2×100 mL)
  2. extractionThe combined extract
  3. washis washed with 1 N HCl (2×10 mL), water
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-db36890a6eb64c089fc51b20a96349ca
出典データセット
uspto-grants-2011_03
特許番号
US07915288B2

関連ノート

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