Benzilic acid → HCID 21521909、化合物

HRID 918304

反応式

HRID 918304 の反応式
[C:1]1([C:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)([OH:11])[C:8]([OH:10])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:18](Br)#[C:19][CH2:20][CH3:21]>CN(C)C=O>[C:1]1([C:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)([O:11][C:2]#[C:1][CH2:6][CH3:5])[C:8]([O:10][C:18]#[C:19][CH2:20][CH3:21])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 6463Benzilic acidHCID 109970821-bromobut-1-yne

生成物 1

HCID 21521909HCID 21521909、化合物収率 122.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Into a suspension of 1.5 g of 66% sodium hydride-paraffin in 20 cc of dimethylformamide was added a solution of 4.5 g of α-phenyl-α-hydroxyphenylacetic acid in 10 cc of dimethylformamide under cooling, and the mixture was stirred for 1 hour. Successively, 5.8 g of butynyl bromide was added thereto and the stirring was continued for 1 hour. The reaction mixture was poured in ice-water, and the resultant was subjected to extraction with ether. The ether extract was washed with an aqueous solution saturated with sodium chloride, and dried over sodium sulfate. Thereafter ether was distilled out and paraffin was removed to obtain 4.0 g of oily 1-butynyl α-phenyl-α-(1-butynyloxy)phenylacetate, nD25 1.5581.

後処理

  1. temperatureunder cooling
  2. waitthe stirring was continued for 1 hour
  3. extractionthe resultant was subjected to extraction with ether
  4. extractionThe ether extract
  5. washwas washed with an aqueous solution saturated with sodium chloride
  6. dry with materialdried over sodium sulfate
  7. distillationThereafter ether was distilled out and paraffin
  8. customwas removed

出典と根拠

ORDレコード
ord-f80841a2d4694390a773a92664bc89e6
出典データセット
uspto-grants-1976_07
特許番号
US03970703

関連ノート

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