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Potassium Carbonate → HCID 14720317, 화합물

HRID 2351986
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HRID 2351986 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chloride2회HCID 516892Sodium BicarbonateHCID 147203163-(3-Trifluoromethylphenylaminomethyl)pyridine

생성물 1

HCID 14720317HCID 14720317, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-79786a6b06ae4ec0866514e6ae50fdba
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04874775

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