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Water → HCID 53703941, 화합물

HRID 1701163
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HRID 1701163 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH:14]([S:16]([CH2:18][C:19]([OH:21])=[O:20])=[O:17])[CH3:15])=[CH:10][CH:9]=1.[C:22]1(C)C=CC(S(O)(=O)=O)=CC=1.O>CO.COC(OC)(C)C>[CH3:22][O:20][C:19](=[O:21])[CH2:18][S:16]([CH:14]([C:11]1[CH:12]=[CH:13][C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])=[CH:9][CH:10]=1)[CH3:15])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 20348737HCID 20348737, 화합물

생성물 1

HCID 53703941HCID 53703941, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 64952,2-Dimethoxypropane용매

실험 절차

1.5 gm (50 millimols) of [1-(2'-fluoro-4-biphenylyl)-ethylsulfinyl]-acetic acid, m.p. 164°-165° C., were dissovled in 3 ml of methanol and 1.2 ml of 2,2-dimethoxypropane, 100 mgm of p-toluenesulfonic acid were added to the solution, and the mixture was allowed to stand for 12 days at room temperature. Then, water was added and the ester was extracted with toluene. The organic extract was washed with water, dried and evaporated, and the residue was purified by chromatography on 75 gm of silicagel (grain size 0.05-0.2 mm) with cyclohexane/ethyl acetate--1/4. The combined ester--containing fractions were evaporated, and the residue was recrystallized from 3 ml of isopropanol. Yield: 800 mgm (50% of theory); m.p. 77°-79° C.

후처리

  1. extractionthe ester was extracted with toluene
  2. extractionThe organic extract
  3. washwas washed with water
  4. customdried
  5. customevaporated
  6. customthe residue was purified by chromatography on 75 gm of silicagel (grain size 0.05-0.2 mm) with cyclohexane/ethyl acetate
  7. additionThe combined ester--containing fractions
  8. customwere evaporated
  9. customthe residue was recrystallized from 3 ml of isopropanol

출처 및 근거

ORD 기록
ord-c44c44ba02b848a28893859cd2041a34
출처 데이터셋
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04191776

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