Water → 1-(3-(Phenylmethoxy)phenyl)ethan-1-one

HRID 225186

反応式

HRID 225186 の反応式
C[Li].[CH2:3]([O:10][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=1)[C:14]([OH:16])=O)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.O1CCC[CH2:21]1.O>CCOCC>[CH3:21][C:14]([C:13]1[CH:17]=[CH:18][CH:19]=[C:11]([O:10][CH2:3][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:12]=1)=[O:16]

参加物

6

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 3092263-(Benzyloxy)benzoic acidHCID 178418348HCID 178418348、化合物

生成物 1

HCID 986891-(3-(Phenylmethoxy)phenyl)ethan-1-one

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Over a period of 1.5 hours, methyl lithium (531 ml. of a 2 molar solution, 1.06 M) is added under a nitrogen atmosphere to a rapidly stirring solution of 3-benzyloxybenzoic acid (116 g., 0.532 M) in ether (250 ml.)-tetrahydrofuran (1400 ml.) maintained at 15°-20° C. After stirring an additional 0.75 hour at 10°-15° C., water (600 ml.) is slowly added keeping the reaction temperature below 20° C. The aqueous layer is separated and extracted with ether (3×250 ml.). The organic phases are combined, washed with saturated sodium chloride solution (4×300 ml.), dried over sodium sulfate, and concentrated under vacuum to give the product as an oil.

後処理

  1. temperaturemaintained at 15°-20° C
  2. customthe reaction temperature below 20° C
  3. customThe aqueous layer is separated
  4. extractionextracted with ether (3×250 ml.)
  5. washwashed with saturated sodium chloride solution (4×300 ml.)
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-2e2ddcc9cc8040d2a238ce1ffe707bee
出典データセット
uspto-grants-1980_11
特許番号
US04235913

関連ノート

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