Benzilic acid → HCID 21521909, 화합물

HRID 918304

반응식

HRID 918304 반응식
[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

참가 물질

4

반응물 2

HCID 6463Benzilic acidHCID 109970821-bromobut-1-yne

생성물 1

HCID 21521909HCID 21521909, 화합물수율 122.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f80841a2d4694390a773a92664bc89e6
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03970703

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