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

HRID 1646188ノート

反応式

HRID 1646188 の反応式
[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]

参加物

4

反応物 2

HCID 76633Phosphonic acid, P-(chloromethyl)-, diethyl esterHCID 178477078HCID 178477078、化合物

生成物 1

HCID 53962055Diethoxyphosphinylmethylthioacetate収率 70.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-13e26aa07aa14c0cb045627c731bee0a
出典データセット
uspto-grants-1993_01
特許番号
US05179085

反応ノート

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