Phosphorodithioate → Methyl 3-thiocarbamoylmethoxybenzoate

HRID 1602496

반응식

HRID 1602496 반응식
P([O-])([O-])([S-])=[S:2].[C:6]([CH2:8][O:9][C:10]1[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=1)[C:13]([O:15][CH3:16])=[O:14])#[N:7]>C(OCC)(=O)C.Cl>[C:6]([CH2:8][O:9][C:10]1[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=1)[C:13]([O:15][CH3:16])=[O:14])(=[S:2])[NH2:7]

참가 물질

4

반응물 2

HCID 177047PhosphorodithioateHCID 14917017Methyl 3-(cyanomethoxy)benzoate

생성물 1

HCID 19611422Methyl 3-thiocarbamoylmethoxybenzoate수율 78%

시약·촉매·용매 1

HCID 21866389Hydrogen chloride-ethyl acetate용매

실험 절차

4 N Hydrogen chloride-ethyl acetate solution (50 ml) and dithiophosphate=O,O-diethyl (4.47 ml, 26.67 mmol) were added in that order to methyl 3-cyanomethoxybenzoate (5.00 g, 26.15 mmol), and the resulting solution was stirred at room temperature for 12 hours. Crystals precipitated in the reaction solution were collected by filtration and washed with diethyl ether to give methyl 3-thiocarbamoylmethoxybenzoate (4.60 g, 78%).

후처리

  1. customCrystals precipitated in the reaction solution
  2. filtrationwere collected by filtration
  3. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-443c714b642b44efbe4a71e33896aeaa
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05981559

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