Toluene → Ethyl 4-(dimethoxyphosphorylmethyl)-3-trifluoromethylbenzoate

HRID 13757

反応式

HRID 13757 の反応式
Br[CH2:2][C:3]1[CH:13]=[CH:12][C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:5][C:4]=1[C:14]([F:17])([F:16])[F:15].C1(C)C=CC=CC=1.[P:25]([O:30]C)([O:28][CH3:29])[O:26][CH3:27]>>[CH3:27][O:26][P:25]([CH2:2][C:3]1[CH:13]=[CH:12][C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:5][C:4]=1[C:14]([F:17])([F:16])[F:15])([O:28][CH3:29])=[O:30]

参加物

4

反応物 3

HCID 1140TolueneHCID 8472Trimethyl phosphiteHCID 23073576Ethyl 4-(bromomethyl)-3-(trifluoromethyl)benzoate

生成物 1

HCID 23145856Ethyl 4-(dimethoxyphosphorylmethyl)-3-trifluoromethylbenzoate

実験手順

6.20 g of ethyl 4-(bromomethyl)-3-trifluoromethylbenzoate (Reference Example 2 (step 2)) was dissolved in 12 ml of trimethyl phosphite and the mixture was heated at reflux for 4 hours under an argon atmosphere. After the completion of the reaction, the operation of adding of toluene to the residue, followed by azeotropic removal of trimethyl phosphite was repeated three times. The residue was purified by silica gel column chromatography to obtain 4.96 g of the objective compound as a yellow oily product.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 4 hours under an argon atmosphere
  3. customAfter the completion of the reaction
  4. customfollowed by azeotropic removal of trimethyl phosphite
  5. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e8b8ff3cc5994df4a322785abc0d4ca2
出典データセット
uspto-grants-2010_06
特許番号
US07728131B2

関連ノート

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