Water → 9-(4-Cyclohexylphenyl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide

HRID 1622599노트

반응식

HRID 1622599 반응식
[CH:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[C:14]([NH2:19])=[N:15][CH:16]=[CH:17][CH:18]=3)=[CH:9][CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].Cl[CH2:23][CH2:24][S:25](Cl)(=[O:27])=[O:26].O>C1COCC1>[CH:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[C:14]4=[N:19][S:25](=[O:27])(=[O:26])[CH2:24][CH2:23][N:15]4[CH:16]=[CH:17][CH:18]=3)=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

6

반응물 4

HCID 962WaterHCID 15385Ethanesulfonylchloride, 2-chloro-HCID 24758Sodium hydrideHCID 655495323-(4-Cyclohexylphenyl)pyridin-2-amine

생성물 1

HCID 668237219-(4-Cyclohexylphenyl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide수율 52.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture of 3-(4-cyclohexylphenyl)pyridin-2-amine (57 mg) in dehydrated THF (5 mL) was added to a mixture of sodium hydride (60%, 45.2 mg) and 2-chloroethanesulfonyl chloride (110 mg) in dehydrated THF (5 mL) under ice-cooling. The reaction mixture was stirred at room temperature overnight, and water was added. The resulting precipitate was collected by filtration, and washed with water and diisopropyl ether to give the title compound (40.3 mg) as a white solid. The obtained solid was crystallized from acetonitrile and diisopropyl ether to give a white solid.

후처리

  1. temperaturecooling
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water and diisopropyl ether

출처 및 근거

ORD 기록
ord-53facc7d759b478b9e45efcdbb5416e5
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08778934B2

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