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Phosphate → Trichloroethyl alpha-amino-diethylphosphonoacetate

HRID 1658002
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HRID 1658002 반응식
C1(C)C=CC(S(O)(=O)=O)=CC=1.[NH2:12][CH:13]([P:22]([O:27][CH2:28][CH3:29])([O:24][CH2:25][CH3:26])=[O:23])[C:14]([O:16][CH2:17][C:18]([Cl:21])([Cl:20])[Cl:19])=[O:15].P([O-])([O-])([O-])=O>C(Cl)Cl>[NH2:12][CH:13]([P:22]([O:24][CH2:25][CH3:26])([O:27][CH2:28][CH3:29])=[O:23])[C:14]([O:16][CH2:17][C:18]([Cl:20])([Cl:21])[Cl:19])=[O:15]
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참가 물질

4

반응물 2

HCID 1061PhosphateHCID 21529973Trichloroethyl alpha-amino-diethylphosphonoacetate p-toluenesulfonate

생성물 1

HCID 21529974Trichloroethyl alpha-amino-diethylphosphonoacetate수율 97.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trichloroethyl α-amino-diethylphosphonoacetate p-toluenesulfonate (1.03 g., 2 mmole) is partitioned between methylene chloride (20 ml.) and aqueous phosphate (4 ml. 1M dipotassium phosphate + 6 ml. water). The aqueous phase (pH 6.8) is separated and extracted with an additional portion of methylene chloride (10 ml.). The combined organic solution is washed with saturated brine (10 ml.), dried over magnesium sulfate, and evaporated in vacuo to give trichloroethyl α-amino-diethylphosphonoacetate (0.67 g.) as a pale yellow oil.

후처리

  1. customThe aqueous phase (pH 6.8) is separated
  2. extractionextracted with an additional portion of methylene chloride (10 ml.)
  3. washThe combined organic solution is washed with saturated brine (10 ml.)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-4abc70a87d9947f190d5ba0223faee9e
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03962224

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