2-Methylbenzamide → Ethyl 2-methyl-benzimidate tetrafluoroborate

HRID 1167347노트

반응식

HRID 1167347 반응식
[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]

참가 물질

4

반응물 2

HCID 107042-MethylbenzamideHCID 2723982Triethyloxonium tetrafluoroborate

생성물 1

HCID 22996236Ethyl 2-methyl-benzimidate tetrafluoroborate수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f07fac63b95c4d7095a5177695724233
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06617346B1

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