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Potassium Hydroxide → HCID 13302029, 화합물

HRID 1709008
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HRID 1709008 반응식
[S:1]1[CH2:6][CH2:5][CH2:4][S:3][C:2]1=[C:7]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=1)[C:8]([O:10]CCCCCCCC)=[O:9].[OH-].[K+]>C(O)C.O>[S:1]1[CH2:6][CH2:5][CH2:4][S:3][C:2]1=[C:7]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:26])([F:27])[F:28])[CH:20]=1)[C:8]([OH:10])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 13302038HCID 13302038, 화합물

생성물 1

HCID 13302029HCID 13302029, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of n-octyl (1,3-dithian-2-ylidene)-(3-trifluoromethylphenyl)-acetate (15 g) in ethanol (375 ml), a 30% solution of potassium hydroxide in water (375 ml) is added. The mixture is refluxed for 2 hours. The solvents are removed in vacuo. Water (500 ml) and ether (500 ml) are added. The water solution is acidified to pH 4 with 5N sulphuric acid. The phases are separated and the water solution is extracted with ether (3×350 ml). The combined organic solutions are dried over magnesium sulphate and the solvent is evaporated in vacuo. The residue is triturated in petrol ether (b.p. 40°-65°) and dried in vacuo to constant weight to give (1,3-dithian-2-ylidene)-(3-trifluoromethylphenyl)-acetic acid, m.p. 165°-166° C.

후처리

  1. temperatureThe mixture is refluxed for 2 hours
  2. customThe solvents are removed in vacuo
  3. additionWater (500 ml) and ether (500 ml) are added
  4. customThe phases are separated
  5. extractionthe water solution is extracted with ether (3×350 ml)
  6. dry with materialThe combined organic solutions are dried over magnesium sulphate
  7. customthe solvent is evaporated in vacuo
  8. customThe residue is triturated in petrol ether (b.p. 40°-65°)
  9. customdried in vacuo to constant weight

출처 및 근거

ORD 기록
ord-6959926cd203474b9710878c749fe859
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04946861

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