Acetic Acid → HCID 14622774, 화합물

HRID 1721937노트

반응식

HRID 1721937 반응식
S1C=CC=C1CC([O-])=O.[K+].[Cl:11][C:12]1[C:17]([Cl:18])=[C:16]([O:19]C)[CH:15]=[CH:14][C:13]=1[C:21]([C:23]1[N:27]([CH2:28][O:29][CH2:30][CH3:31])[N:26]=[CH:25][CH:24]=1)=[O:22].O.C(O)(=O)C>CS(C)=O>[Cl:18][C:17]1[C:12]([Cl:11])=[C:13]([C:21]([C:23]2[N:27]([CH2:28][O:29][CH2:30][CH3:31])[N:26]=[CH:25][CH:24]=2)=[O:22])[CH:14]=[CH:15][C:16]=1[OH:19]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 14622785HCID 14622785, 화합물HCID 23696799Potassium 2-thienylacetate

생성물 1

HCID 14622774HCID 14622774, 화합물수율 71.3%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

9.45 g of potassium thiolacetate are added to a solution of 5.45 g of (2,3-dichloro-4-methoxyphenyl)(1-ethoxymethyl-5-pyrazolyl)methanone in dimethylsulfoxide and the mixture is stirred at 90°-100° C. under argon gas atmosphere for 4 hours. After cooling the solution, cold water is added thereto, and the mixture is adjusted to pH 5-6 with acetic acid and then extracted with ethyl acetate. The extract is washed with water, dried and evaporated to remove solvent. The residue is purified by silica gel column chromatography to give 3.72 g of 2,3-dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenol.

후처리

  1. additionis added
  2. extractionextracted with ethyl acetate
  3. washThe extract is washed with water
  4. customdried
  5. customevaporated
  6. customto remove solvent
  7. customThe residue is purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-aa4f7bde85d64daa844eb84d52806c60
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853404

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