Ethyl Acetate → Benzyl (3-hydroxycyclohexyl)carbamate

HRID 1013812ノート

反応式

HRID 1013812 の反応式
[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH:4]([NH2:8])[CH2:3]1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C.Cl[C:22]([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23]>O>[CH2:25]([O:24][C:22](=[O:23])[NH:8][CH:4]1[CH2:5][CH2:6][CH2:7][CH:2]([OH:1])[CH2:3]1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 10387Benzyl chloroformateHCID 11430Potassium CarbonateHCID 112404593-Aminocyclohexanol

生成物 1

HCID 14476840Benzyl (3-hydroxycyclohexyl)carbamate収率 88.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Treat a mixture of 3-hydroxycyclohexyl amine (10 g, 86.96 mmol), potassium carbonate (18 g, 130 mmol), ethyl acetate (150 mL) and water (70 mL) with benzyl chloroformate (22.17 g, 130 mmol). Stir the reaction at room temperature for 12 hours. Separate the organic layer, dry the organic over sodium sulfate, filter and concentrate. Add diethyl ether to the residuer. Filter the resulting white precipitate and air dry to afford 19.1 g of the title compound (88%). MS (m/z): 250 (M+).

後処理

  1. additionTreat
  2. customthe reaction at room temperature for 12 hours
  3. customSeparate the organic layer
  4. dry with materialdry the organic over sodium sulfate
  5. filtrationfilter
  6. concentrationconcentrate
  7. filtrationFilter the resulting white precipitate and air
  8. customdry

出典と根拠

ORDレコード
ord-804318bcbfbb46449e650c709fde728c
出典データセット
uspto-grants-2011_07
特許番号
US07981918B2

反応ノート

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