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

HRID 1621098

반응식

HRID 1621098 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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)+

후처리

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

출처 및 근거

ORD 기록
ord-3e555c6bb8984d90a54f7ba5a9148bbd
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772510B2

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