Acetic Acid → HCID 14622774、化合物

HRID 1721937ノート

反応式

HRID 1721937 の反応式
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]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 14622785HCID 14622785、化合物HCID 23696799Potassium 2-thienylacetate

生成物 1

HCID 14622774HCID 14622774、化合物収率 71.3%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aa4f7bde85d64daa844eb84d52806c60
出典データセット
uspto-grants-1989_08
特許番号
US04853404

反応ノート

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