Water → Acetamide, N-(2-methoxyphenyl)-

HRID 1084983

반응식

HRID 1084983 반응식
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9](=[O:11])[CH3:10].C[O-].[Na+].[OH:15][C:16]1C=CC=C2C=1N=CC=C2.O>CO.C(OCC)(=O)C>[C:9]([NH:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[O:15][CH3:16])(=[O:11])[CH3:10]

참가 물질

7

반응물 4

HCID 962WaterHCID 19238-HydroxyquinolineHCID 1364162'-BromoacetanilideHCID 10942334Sodium Methoxide

생성물 1

HCID 7135Acetamide, N-(2-methoxyphenyl)-수율 945.4%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 8857Ethyl Acetate용매

실험 절차

Then, 2.14 g of the 2-bromo-1-acetylaminobenzene was added to a solution containing 2.3 ml of a 28% methanol solution of sodium methoxide, 100 mg of cuprous chloride, and 145 mg of 8-hydroxyquinoline in 40 ml of methanol, and the mixture was heated under reflux for 50 minutes. After cooling with water, ethyl acetate was added thereto, and the resulting mixture was washed with water and dried over Glauber's salt. The solvent was distilled off, and the obtained crude crystals were recrystallized from an n-hexane/ethyl acetate solvent mixture, to obtain 1.56 g (yield: 95%) of the desired compound. The spectrum data of the compound was in agreement with the spectrum data of the separately synthesized reference compound.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 50 minutes
  3. additionwas added
  4. washthe resulting mixture was washed with water
  5. dry with materialdried over Glauber's salt
  6. distillationThe solvent was distilled off
  7. customthe obtained crude crystals
  8. customwere recrystallized from an n-hexane/ethyl acetate solvent mixture

출처 및 근거

ORD 기록
ord-754bd2a780e04efca6334d8b524c3684
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05006660

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