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2-(Chloromethyl)-5-methyl-1,2-oxazol-3(2H)-one → HCID 20332918, 화합물

HRID 1706870
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반응식

HRID 1706870 반응식
Cl[CH2:2][N:3]1[C:7](=[O:8])[CH:6]=[C:5]([CH3:9])[O:4]1.[P:10]([S-:20])([O:16][CH2:17][CH2:18][CH3:19])([O:12][CH2:13][CH2:14][CH3:15])=[S:11].[K+]>CC(C)=O>[P:10]([S:20][CH2:2][N:3]1[C:7](=[O:8])[CH:6]=[C:5]([CH3:9])[O:4]1)(=[S:11])([O:16][CH2:17][CH2:18][CH3:19])[O:12][CH2:13][CH2:14][CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 203329192-(Chloromethyl)-5-methyl-1,2-oxazol-3(2H)-oneHCID 23678805Potassium O,O-dipropyl dithiophosphate

생성물 1

HCID 20332918HCID 20332918, 화합물수율 73.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 1.48 g of the 2-chloromethyl-5-methyl-4-isoxazolin-3-one thus obtained in 30 ml of acetone were added 2.52 g of crystalline potassium O,O-di-n-propyl dithiophosphate, and the resulting mixture was then stirred for 1 hour at ambient temperature. The acetone was then evaporated off and the residue was purified by column chromatography through silica gel eluted with a 20:1 by volume mixture of benzene and acetone. There were obtained 2.39 g (73.5% of theory) of O,O-di-n-propyl S-(5-methyl-3-oxo-4-isoxazolin-2-ylmethyl) phosphorodithioate, in the form of a pale yellow oil, n20D =1.5314.

후처리

  1. customThe acetone was then evaporated off
  2. customthe residue was purified by column chromatography through silica gel
  3. washeluted with a 20:1 by volume mixture of benzene and acetone

출처 및 근거

ORD 기록
ord-ee50bbb9cbb443cdae477a948f326e8d
출처 데이터셋
uspto-grants-1980_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04209512

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