Phosphorodithioate → Methyl 3-thiocarbamoylmethoxybenzoate

HRID 1602496

反応式

HRID 1602496 の反応式
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]

参加物

4

反応物 2

HCID 177047PhosphorodithioateHCID 14917017Methyl 3-(cyanomethoxy)benzoate

生成物 1

HCID 19611422Methyl 3-thiocarbamoylmethoxybenzoate収率 78%

試薬・触媒・溶媒 1

HCID 21866389Hydrogen chloride-ethyl acetate溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-443c714b642b44efbe4a71e33896aeaa
出典データセット
uspto-grants-1999_11
特許番号
US05981559

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