Benzyl chloroformate → Carbamic acid, (6-hydroxyhexyl)-, phenylmethyl ester

HRID 376105

反応式

HRID 376105 の反応式
[CH2:1]([O:8][C:9](Cl)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][OH:19].C(=O)([O-])O.[Na+]>CC(C)=O.O>[CH2:1]([O:8][C:9]([NH:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][OH:19])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 10387Benzyl chloroformateHCID 199606-Amino-1-hexanolHCID 516892Sodium Bicarbonate

生成物 1

HCID 4184071Carbamic acid, (6-hydroxyhexyl)-, phenylmethyl ester

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

7.06 ml (47 mmol) of chloroformic acid benzyl ester are added dropwise to a solution of 5.52 g (47 mmol) of 6-aminohexan-1-ol and 3.95 g (47 mmol) of sodium hydrogen carbonate in 100 ml of acetone and 50 ml of water. The mixture is stirred at room temperature for 18 hours and concentrated to approximately 70 ml, and the white precipitate is filtered off, washed with approximately 20 ml of water, taken up in 250 ml of methylene chloride and dried over magnesium sulfate; the magnesium sulfate is filtered off and the residue is concentrated to dryness by evaporation. 6-(N-benzyloxycarbonylamino)hexan-1-ol is obtained in the form of white crystals having a melting point of 58°-60°.

後処理

  1. concentrationconcentrated to approximately 70 ml
  2. filtrationthe white precipitate is filtered off
  3. washwashed with approximately 20 ml of water
  4. dry with materialdried over magnesium sulfate
  5. filtrationthe magnesium sulfate is filtered off
  6. concentrationthe residue is concentrated to dryness by evaporation

出典と根拠

ORDレコード
ord-936b247750754cecb261202c8f1c2d6c
出典データセット
uspto-grants-1996_01
特許番号
US05488140

関連ノート

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