Water → Phenacyl 4-hydroxymethylphenoxyacetate

HRID 865444노트

반응식

HRID 865444 반응식
[OH:1][CH2:2][C:3]1[CH:13]=[CH:12][C:6]([O:7][CH2:8][C:9]([OH:11])=[O:10])=[CH:5][CH:4]=1.Br[CH2:15][C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:17].C(N(CC)CC)C.O>CN(C=O)C>[OH:1][CH2:2][C:3]1[CH:13]=[CH:12][C:6]([O:7][CH2:8][C:9]([O:11][CH2:15][C:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[O:17])=[O:10])=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6259Phenacyl bromideHCID 8471TriethylamineHCID 1942914-Hydroxymethylphenoxyacetic acid

생성물 1

HCID 11954711Phenacyl 4-hydroxymethylphenoxyacetate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

182 g of 4-hydroxymethylphenoxyacetic acid and 199 g of α-bromoacetophenone are dissolved in 600 ml of dry DMF, and then, at 0° C., 138 ml of triethylamine are rapidly added dropwise. The mixture is allowed to reach room temperature, and is stirred overnight. The DMF solution is poured into 3.5 1 of water, and the aqueous phase is extracted with ethyl acetate. The organic phase is washed with water, dried over sodium sulfate and concentrated. The product precipitates out on evaporation. It is filtered off with suction, washed with ethyl acetate/n-hexane 1:1 and dried under high vacuum.

후처리

  1. customto reach room temperature
  2. extractionthe aqueous phase is extracted with ethyl acetate
  3. washThe organic phase is washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe product precipitates out on evaporation
  7. filtrationIt is filtered off with suction
  8. washwashed with ethyl acetate/n-hexane 1:1
  9. customdried under high vacuum

출처 및 근거

ORD 기록
ord-1d4d0bea01b145a0afbc224b7d555354
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05565606

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