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Benzyl chloroformate → HCID 178523374, 화합물

HRID 1612669
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HRID 1612669 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][PH:5](=[O:7])[OH:6].[OH-].[Na+].Cl[C:11]([O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:12]>O>[CH2:14]([O:13][C:11]([NH:1][CH2:2][CH2:3][CH2:4][PH:5](=[O:6])[OH:7])=[O:12])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10387Benzyl chloroformateHCID 14798Sodium HydroxideHCID 1219563-Aminopropylphosphinic acid

생성물 1

HCID 178523374HCID 178523374, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 5.0 g of 3-aminopropylphosphinic acid in 200 ml of water is cooled to 5°, and the pH adjusted to 9.5 with 2 molar sodium hydroxide solution. To this mixture is added 6.8 g of benzyl chloroformate whilst maintaining the pH and temperature. After the addition is complete the mixture is stirred for 3 hours at pH 9.5 at room temperature and left to stand overnight. The mixture is then extracted with 100 ml of ether and the aqueous layer stirred at 5° with an equal volume of chloroform. The mixture is acidified to pH 2, the chloroform layer separated, dried over magnesium sulfate and the solvent evaporated under reduced pressure. The oily product is triturated with ether to give a white solid, 3-(N-benzyloxycarbonylamino)propylphosphinic acid, m.p. 53°-55°, 31P-NMR: δ=+36.6 ppm (CDCl3).

후처리

  1. temperaturewhilst maintaining the pH and temperature
  2. additionAfter the addition
  3. waitleft
  4. waitto stand overnight
  5. extractionThe mixture is then extracted with 100 ml of ether
  6. stirringthe aqueous layer stirred at 5° with an equal volume of chloroform
  7. customthe chloroform layer separated
  8. dry with materialdried over magnesium sulfate
  9. customthe solvent evaporated under reduced pressure
  10. customThe oily product is triturated with ether

출처 및 근거

ORD 기록
ord-1262cd8b72c94c4090b7f57ff6ce8743
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05190933

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