Water → Diethyl 4-isothiocyanatobenzylphosphonate

HRID 25512

반응식

HRID 25512 반응식
[C:1](Cl)(Cl)=[S:2].[NH2:5][C:6]1[CH:20]=[CH:19][C:9]([CH2:10][P:11](=[O:18])([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])=[CH:8][CH:7]=1.C(=O)(O)[O-].[Na+].O>ClCCl>[N:5]([C:6]1[CH:7]=[CH:8][C:9]([CH2:10][P:11](=[O:18])([O:12][CH2:13][CH3:14])[O:15][CH2:16][CH3:17])=[CH:19][CH:20]=1)=[C:1]=[S:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 10040ThiophosgeneHCID 88358Diethyl p-aminobenzylphosphonateHCID 516892Sodium Bicarbonate

생성물 1

HCID 22568434Diethyl 4-isothiocyanatobenzylphosphonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Thiophosgene (4.1 mL, 54 mmol) was added al at once to a mixture of diethyl 4-aminobenzylphosphonate (12.04 g, 50 mmol), sodium bicarbonate (8.33 g, 99 mmol), water (100 mL), and dichloromethane (250 mL), and the mixture was stirred at room temperature for about 2 hours. The organic and aqueous layers were separated, the organic layer dried over magnesium sulfate, filtered, and concentrated to give the product isothiocyanate as a brown oil. This was used directly in the next step.

후처리

  1. customThe organic and aqueous layers were separated
  2. dry with materialthe organic layer dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2c8f5600ae6f41b9984d67f20d309d62
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858739B2

연결된 노트

불러오는 중…