Benzyl Bromide → 2-Amino-2'-benzyloxy-5-chlorobenzophenone

HRID 1799

反応式

HRID 1799 の反応式
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[OH:12])=[O:5].C(=O)([O-])[O-].[K+].[K+].[CH2:24](Br)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>CN(C)C=O>[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:5]

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 5264882-Amino-5-chloro-2'-hydroxybenzophenone

生成物 1

HCID 541754792-Amino-2'-benzyloxy-5-chlorobenzophenone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In 30 ml of N,N-dimethylformamide was dissolved 5.0 g of 2-amino-5-chloro-2'-hydroxybenzophenone, as obtained in Example 123 (1), to which were added 4.2 g of potassium carbonate and 2.9 ml of benzyl bromide; the mixture was then stirred for 2 hours at room temperature. The mixture was subjected to extraction with 150 ml of water and 200 ml of ethyl acetate, and the ethyl acetate layer was washed with water, dried over anhydrous magnesium sulfate, and distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1 to 5:1) to yield 6.4 g of 2-amino-2'-benzyloxy-5-chlorobenzophenone as prism crystals, m.p. 110° to 111° C.

後処理

  1. extractionThe mixture was subjected to extraction with 150 ml of water and 200 ml of ethyl acetate
  2. washthe ethyl acetate layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationdistilled off under reduced pressure
  5. customThe residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1 to 5:1)

出典と根拠

ORDレコード
ord-c2eabdf1be4f4a81a4b9a839ae6cea53
出典データセット
uspto-grants-1998_03
特許番号
US05726306

関連ノート

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