Water → Tak-137

HRID 1405869노트

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HRID 1405869 반응식
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:15]([NH2:20])=[N:16][CH:17]=[CH:18][CH:19]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:22][CH2:23][S:24](Cl)(=[O:26])=[O:25].O>CN(C)C(=O)C>[O:1]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:15]3=[N:20][S:24](=[O:26])(=[O:25])[CH2:23][CH2:22][N:16]3[CH:17]=[CH:18][CH:19]=2)=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 15385Ethanesulfonylchloride, 2-chloro-HCID 655512093-(4-Phenoxyphenyl)pyridin-2-amine

생성물 1

HCID 56649286Tak-137수율 85.7%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매2회

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온도
60 °C

실험 절차

A solution of 3-(4-phenoxyphenyl)pyridin-2-amine (301 mg) in N,N-dimethylacetoamide (3 mL) was added dropwise to 2-chloroethanesulfonyl chloride (382 mg) and additional N,N-dimethylacetoamide (2 mL) was used to complete the addition of above solution. After being stirred at 60° C. for 4 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 THF (3 mL), and dried in vacuo at 60° C. to give the title compound (346.7 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 THF (3 mL)
  6. customdried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-efa28ae00b3c4eb98d1cf79a00dafcf5
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08916551B2

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