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

HRID 1084983

反応式

HRID 1084983 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-754bd2a780e04efca6334d8b524c3684
出典データセット
uspto-grants-1991_04
特許番号
US05006660

関連ノート

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