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Water → N-(1-(4-hydroxymethylphenyl)-1-methylethyl)acetamide

HRID 1282161
ノート
印刷プレビュー

反応式

HRID 1282161 の反応式
[C:1]([NH:4][C:5]([C:8]1[CH:17]=[CH:16][C:11]([C:12](OC)=[O:13])=[CH:10][CH:9]=1)([CH3:7])[CH3:6])(=[O:3])[CH3:2].[BH4-].[Li+].O>O1CCCC1>[OH:13][CH2:12][C:11]1[CH:10]=[CH:9][C:8]([C:5]([NH:4][C:1](=[O:3])[CH3:2])([CH3:7])[CH3:6])=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 4148881Lithium borohydrideHCID 18423021Methyl 4-(1-acetamido-1-methylethyl)benzoate

生成物 1

HCID 18423112N-(1-(4-hydroxymethylphenyl)-1-methylethyl)acetamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl 4-(1-acetamido-1-methylethyl)benzoate (37.14g) in tetrahydrofuran (370 ml) was added lithium borohydride (6.88 g) and the mixture was refluxed for 19 hr. The reaction mixture was poured into water (1000 ml) and extracted with ethyl acetate (1000 ml). The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated and the obtained residue was recrystallized from ethyl acetate to give the title compound (18.24 m.p.=126-129° C.

後処理

  1. temperaturethe mixture was refluxed for 19 hr
  2. extractionextracted with ethyl acetate (1000 ml)
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe obtained residue was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-eca1881ab8af41a0a27c81f76b283411
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06455528B1

反応ノート

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