2-Methylbenzamide → Ethyl 2-methyl-benzimidate tetrafluoroborate

HRID 1167347ノート

反応式

HRID 1167347 の反応式
[C:1]1([CH3:10])[C:2]([C:7]([NH2:9])=[O:8])=[CH:3][CH:4]=[CH:5][CH:6]=1.[F:11][B-:12]([F:15])([F:14])[F:13].[CH2:16]([O+](CC)CC)[CH3:17]>C(Cl)Cl>[F:11][B-:12]([F:15])([F:14])[F:13].[CH3:10][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=[NH:9])[O:8][CH2:16][CH3:17]

参加物

4

反応物 2

HCID 107042-MethylbenzamideHCID 2723982Triethyloxonium tetrafluoroborate

生成物 1

HCID 22996236Ethyl 2-methyl-benzimidate tetrafluoroborate収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a degassed suspension of o-toluamide (1.35 g, 9.788 mmol) in methylene chloride (5 mL) was added triethyloxonium tetrafluoroborate (9.788 mL, 9.788 mmol, 1 M in methylene chloride). After the clear solution was stirred at room temperature overnight, it was concentrated in vacuo. The residue was triturated in methylene chloride and diethyl ether. The white solid was filtered off and washed with diethyl ether to afford ethyl 2-methyl-benzimidate tetrafluoroborate (1.4 g, 80%). It was used without further purification.

後処理

  1. concentrationit was concentrated in vacuo
  2. customThe residue was triturated in methylene chloride
  3. filtrationThe white solid was filtered off
  4. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-f07fac63b95c4d7095a5177695724233
出典データセット
uspto-grants-2003_09
特許番号
US06617346B1

反応ノート

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