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Potassium Carbonate → HCID 178458881、化合物

HRID 703362
ノート
印刷プレビュー

反応式

HRID 703362 の反応式
[OH:1][C:2]1[CH2:7][CH:6]([C:8]2[CH:13]=[CH:12][C:11]([SH:14])=[CH:10][CH:9]=2)[CH2:5][C:4](=[O:15])[C:3]=1[C:16](=[O:19])[CH2:17][CH3:18].F[C:21]1[C:26]([F:27])=[CH:25][C:24]([C:28]([F:31])([F:30])[F:29])=[CH:23][N:22]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C.O.C(Cl)Cl>[C:16]([C:3]1[C:2](=[O:1])[CH2:7][CH:6]([C:8]2[CH:13]=[CH:12][C:11]([S:14][C:21]3[C:26]([F:27])=[CH:25][C:24]([C:28]([F:31])([F:29])[F:30])=[CH:23][N:22]=3)=[CH:10][CH:9]=2)[CH2:5][C:4]=1[OH:15])(=[O:19])[CH2:17][CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 134215472,3-Difluoro-5-(trifluoromethyl)pyridineHCID 178458882HCID 178458882、化合物

生成物 1

HCID 178458881HCID 178458881、化合物収率 89.5%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6342Acetonitrile溶媒
HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4.0 g (0.0145 mol) of 3-hydroxy-5-(4-mercaptophenyl)-2-propionyl-cyclohex-2-en-1-one in 50 mL of acetonitrile was added 3.90 g (0.0212 mol) of 2,3-difluoro-5-(trifluoromethyl)pyridine and 4.50 g (0.0326 mol) of powdered potassium carbonate. The mixture was stirred one hour at ambient temperature and then heated at reflux for 1.5 hours and cooled to room temperature. The reaction mixture was diluted with 150 mL of water and 150 mL of methylene chloride. The organic layer was separated, washed twice with 150 mL portions of water and dried over Na2SO4. The solvent was removed in vacuo leaving 5.7 g of the crude product which was purified by column chromatography using methylene chloride as the eluent. Recrystallization of the crude from ethanol gave the above named product in a yield of 2.25 g (35 percent of theoretical). The product melted at 152°-154° C.; 1H NMR (CDCl3): δ 1.10 (t, 3H, CH3CH2 --), 2.55-3.65 (m, 7H, ring protons and CH3CH2 --), 7.15-8.50 (m, 6H, ArH), 18.2 (s, 1H, OH).

後処理

  1. temperatureheated
  2. temperatureat reflux for 1.5 hours
  3. temperaturecooled to room temperature
  4. customThe organic layer was separated
  5. washwashed twice with 150 mL portions of water
  6. dry with materialdried over Na2SO4
  7. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-595bb586452c4d119203a00a416e7987
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04983211

反応ノート

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