Phosphonic acid, P-(chloromethyl)-, diethyl ester → Diethoxyphosphinylmethylthioacetate

HRID 1646188노트

반응식

HRID 1646188 반응식
[C:1]([O-:4])(=[S:3])[CH3:2].C([N+](CCCC)(CCCC)CCCC)CCC.Cl[CH2:23][P:24](=[O:31])([O:28][CH2:29][CH3:30])[O:25][CH2:26][CH3:27]>O1CCCC1>[CH2:26]([O:25][P:24]([CH2:23][O:4][C:1](=[S:3])[CH3:2])([O:28][CH2:29][CH3:30])=[O:31])[CH3:27]

참가 물질

4

반응물 2

HCID 76633Phosphonic acid, P-(chloromethyl)-, diethyl esterHCID 178477078HCID 178477078, 화합물

생성물 1

HCID 53962055Diethoxyphosphinylmethylthioacetate수율 70.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of tetra-n-butylammonium thioacetate (12.8 g, 0.041 mol) and diethyl chloromethylphosphonate (5 g, 0.027 mol) is stirred in tetrahydrofuran (30 ml) overnight at room temperature. After evaporation of the solvent, the residue is purified by silica gel chromatography (2:1 heptane:acetone as eluant) to give diethoxyphosphinylmethylthioacetate (4.3 g). 1H-NMR: 4H, m, 4.20-4.11 ppm; 2H, d, 3.23; 3H, s, 2.40; 6H, m, 1.33.

후처리

  1. customAfter evaporation of the solvent
  2. customthe residue is purified by silica gel chromatography (2:1 heptane:acetone as eluant)

출처 및 근거

ORD 기록
ord-13e26aa07aa14c0cb045627c731bee0a
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05179085

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