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Water → 2-Thien-2-yl-3-oxo-4-(-3-trifluoromethylphenyl)-5-methylamino-2,3-dihydrofuran

HRID 485617
ノート
印刷プレビュー

反応式

HRID 485617 の反応式
[OH-].[Na+].O.[S:4]1[CH:8]=[CH:7][CH:6]=[C:5]1[CH:9]1[C:13](=[O:14])[C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=2)=[C:11]([NH2:25])[O:10]1.S(OC)(O[CH3:30])(=O)=O>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C(Cl)Cl>[S:4]1[CH:8]=[CH:7][CH:6]=[C:5]1[CH:9]1[C:13](=[O:14])[C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:22])([F:23])[F:24])[CH:16]=2)=[C:11]([NH:25][CH3:30])[O:10]1
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 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 136911642-Thien-2-yl-3-oxo-4-(3-trifluoromethylphenyl)-5-amino-2,3-dihydrofuran

生成物 1

HCID 136911652-Thien-2-yl-3-oxo-4-(-3-trifluoromethylphenyl)-5-methylamino-2,3-dihydrofuran

試薬・触媒・溶媒 2

HCID 66133
Benzyl triethylammonium chloride
触媒
HCID 6344Dichloromethane溶媒2 回

実験手順

In this example about 0.36 g of solid sodium hydroxide was dissolved in a small amount of water and then added to 100 ml of methylene chloride containing 1.4 g of 2-thien-2-yl-3-oxo-4-(3-trifluoromethylphenyl)-5-amino-2,3-dihydrofuran. 0.20 g of benzyltriethylammonium chloride was added and then a mixture containing 0.84 ml of dimethyl sulfate in about 5.0 ml of methylene chloride was slowly added at room temperature. The mixture was stirred at room temperature for about one hour and then washed twice with water, twice with 1N. aqueous hydrochloric acid, twice with sodium bicarbonate, dried over magnesium sulfate and then concentrated by evaporation under vacuum. The residue was then triturated in a mixture of ethyl ether and petroleum ether affording 1.4 g of the title compound.

後処理

  1. additionwas slowly added at room temperature
  2. washwashed twice with water, twice with 1N
  3. dry with materialaqueous hydrochloric acid, twice with sodium bicarbonate, dried over magnesium sulfate
  4. concentrationconcentrated by evaporation under vacuum
  5. customThe residue was then triturated in a mixture of ethyl ether and petroleum ether affording 1.4 g of the title compound

出典と根拠

ORDレコード
ord-fb0b3a778d7b41f0a7b7a86c4e68deb0
出典データセット
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04537623

反応ノート

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