O,O-Diethyl dithiophosphate → 3-(1,3-dioxo-2,3-dihydro-1H-isoindol-2-yl)propanethioamide

HRID 1621098

反応式

HRID 1621098 の反応式
[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[CH2:12][CH2:13][C:14]#[N:15].C(OP(=S)(OCC)[SH:20])C>O>[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[CH2:12][CH2:13][C:14]([NH2:15])=[S:20]

参加物

4

反応物 2

HCID 9274O,O-Diethyl dithiophosphateHCID 3521693-(1,3-dioxo-2,3-dihydro-1H-isoindol-2-yl)propanenitrile

生成物 1

HCID 9696783-(1,3-dioxo-2,3-dihydro-1H-isoindol-2-yl)propanethioamide収率 91%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A suspension of 3-(1,3-dioxoisoindolin-2-yl)-propionitrile (2 g, 9.99 mmol) and dithiophosphoric acid O,O′-diethyl ester (2.05 g, 1.74 mL, 11.0 mmol) in water (4 mL) was irradiated at 80° C. for 10 min. The obtained suspension was diluted with water (5 mL), filtered, washed with water and dried in vacuo to give the product as light yellow solid (2.13 g, 9.09 mmol, 91.0%) which was used without further purification for the next step. MS: M=235.1 (M+H)+

後処理

  1. customwas irradiated at 80° C. for 10 min
  2. filtrationfiltered
  3. washwashed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-3e555c6bb8984d90a54f7ba5a9148bbd
出典データセット
uspto-grants-2014_07
特許番号
US08772510B2

関連ノート

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