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Potassium Carbonate → HCID 14720317、化合物

HRID 2351986
ノート
印刷プレビュー

反応式

HRID 2351986 の反応式
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:4]=[C:5]([NH:9][CH2:10][C:11]2[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=2)[CH:6]=[CH:7][CH:8]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:25][S:26](Cl)(=[O:28])=[O:27].C(=O)(O)[O-].[Na+]>ClCCl>[N:13]1[CH:14]=[CH:15][CH:16]=[C:11]([CH2:10][N:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:17])[F:18])[CH:4]=2)[S:26]([CH3:25])(=[O:28])=[O:27])[CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chloride2 回HCID 516892Sodium BicarbonateHCID 147203163-(3-Trifluoromethylphenylaminomethyl)pyridine

生成物 1

HCID 14720317HCID 14720317、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 3.8 g. portion of 3-(3-trifluoromethylphenylaminomethyl)pyridine was dissolved in 15 ml. of dichloromethane and to it was added 2.7 g. of potassium carbonate and 1.6 ml. of methanesulfonyl chloride. The mixture was stirred at ambient temperature overnight, and at a gentle reflux for another day. Another 1.6 ml. of methanesulfonyl chloride was added, and the mixture was stirred under reflux for 3 days more. It was then cooled, and diluted with 20 ml. of aqueous sodium bicarbonate. The organic phase was separated, washed with water, dried and evaporated under vacuum. The residue was triturated with diethyl ether and petroleum ether, and dried to give 4.7 g. of the desired product, m.p. 106°-110°.

後処理

  1. temperatureat a gentle reflux for another day
  2. stirringthe mixture was stirred
  3. temperatureunder reflux for 3 days more
  4. temperatureIt was then cooled
  5. additiondiluted with 20 ml
  6. customThe organic phase was separated
  7. washwashed with water
  8. customdried
  9. customevaporated under vacuum
  10. customThe residue was triturated with diethyl ether and petroleum ether
  11. customdried
  12. customto give 4.7 g

出典と根拠

ORDレコード
ord-79786a6b06ae4ec0866514e6ae50fdba
出典データセット
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04874775

反応ノート

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