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Dichloromethane → 6-(Dimethoxythiophosphoryl)hexanoic acid tert-butyl ester

HRID 496325
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인쇄 미리보기

반응식

HRID 496325 반응식
C[S:2][P:3]([O-:6])[O:4][CH3:5].[C:7]([O:11][C:12](=[O:19])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]Br)([CH3:10])([CH3:9])[CH3:8].[OH-].[Na+].Cl[CH2:23]Cl>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.O>[C:7]([O:11][C:12](=[O:19])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][P:3]([O:6][CH3:23])([O:4][CH3:5])=[S:2])([CH3:10])([CH3:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 11550568Tert-butyl 6-bromohexanoateHCID 86596782Dimethyl thiophosphite

생성물 1

HCID 860326996-(Dimethoxythiophosphoryl)hexanoic acid tert-butyl ester

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride
촉매
HCID 962Water용매

실험 절차

A solution of dimethylthiophosphite (4.56 g, 36.2 mmol), 6-bromohexanoic acid tert-butyl ester (100 g, 39.8 mmol) and triethylbenzylammonium chloride (0.82 g, 3.62 mmol) in dichloromethane (100 mL) was cooled on an ice bath and a solution of sodium hydroxide (14.5 g, 0.362 mol) in water (14.5 mL) was added slowly with vigorous stirring. The ice bath was removed and the mixture stirred for 3 days before being washed with water, dried (magnesium sulfate), and the solvent removed under reduced pressure to give crude 6-(dimethoxythiophosphoryl)hexanoic acid tert-butyl ester (8.00 g).

후처리

  1. customThe ice bath was removed
  2. washbefore being washed with water
  3. dry with materialdried (magnesium sulfate)
  4. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-d2e8daade79b4195a1d79c927e61d125
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06943267B1

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