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

HRID 1622806
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HRID 1622806 반응식
Cl[CH2:2][CH2:3][S:4](Cl)(=[O:6])=[O:5].[CH:8]1([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[C:22]([NH2:27])=[N:23][CH:24]=[CH:25][CH:26]=3)=[CH:17][CH:16]=2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.O>CN(C)C(=O)C>[CH:8]1([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[C:22]4=[N:27][S:4](=[O:6])(=[O:5])[CH2:3][CH2:2][N:23]4[CH:24]=[CH:25][CH:26]=3)=[CH:17][CH:16]=2)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1
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참가 물질

5

반응물 3

HCID 962WaterHCID 15385Ethanesulfonylchloride, 2-chloro-HCID 667487623-(4-(Cyclohexyloxy)phenyl)pyridin-2-amine

생성물 1

HCID 566558349-[4-(Cyclohexyloxy)phenyl]-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide수율 85.1%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매3회

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온도
60 °C

실험 절차

A solution of 2-chloroethanesulfonyl chloride (381 mg) in N,N-dimethylacetoamide (2 mL) was added dropwise to a suspension of 3-[4-(cyclohexyloxy)phenyl]pyridin-2-amine (301 mg) in N,N-dimethylacetoamide (2 ml) and additional N,N-dimethylacetoamide (1 mL) was used to complete the addition of above solution. After being stirred at 60° C. for 3 hr, the mixture was cooled to room temperature. Water (10 mL) was added dropwise to the reaction mixture and the whole was stirred at room temperature for 0.5 hr. The precipitate was collected by filtration, washed with water (10 mL) and diisopropyl ether (3 ml), and dried in vacuo at 60° C. to give the title compound (342 mg) as an off-white powder.

후처리

  1. additionthe addition of above solution
  2. temperaturethe mixture was cooled to room temperature
  3. stirringthe whole was stirred at room temperature for 0.5 hr
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water (10 mL) and diisopropyl ether (3 ml)
  6. customdried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-3f9a051ad44142e9aa020a891c47637c
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08778934B2

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