4-Aminophenylsulphur pentafluoride → 2-cyclopropyl-5-methyl-N-[4-(pentafluoro-lambda6-sulfanyl)phenyl][1,2,4]triazolo[1,5-a]pyrimidin-7-amine

HRID 591247노트

반응식

HRID 591247 반응식
Cl[C:2]1[N:7]2[N:8]=[C:9]([CH:11]3[CH2:13][CH2:12]3)[N:10]=[C:6]2[N:5]=[C:4]([CH3:14])[CH:3]=1.[NH2:15][C:16]1[CH:21]=[CH:20][C:19]([S:22]([F:27])([F:26])([F:25])([F:24])[F:23])=[CH:18][CH:17]=1>C(O)C>[CH:11]1([C:9]2[N:10]=[C:6]3[N:5]=[C:4]([CH3:14])[CH:3]=[C:2]([NH:15][C:16]4[CH:21]=[CH:20][C:19]([S:22]([F:27])([F:23])([F:24])([F:25])[F:26])=[CH:18][CH:17]=4)[N:7]3[N:8]=2)[CH2:13][CH2:12]1

참가 물질

4

반응물 2

HCID 27791904-Aminophenylsulphur pentafluorideHCID 533918677-Chloro-2-cyclopropyl-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidine

생성물 1

HCID 513475462-cyclopropyl-5-methyl-N-[4-(pentafluoro-lambda6-sulfanyl)phenyl][1,2,4]triazolo[1,5-a]pyrimidin-7-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of Intermediate 20 (0.04 g, 0.192 mmol) in ethanol (2.5 mL), 4-aminophenylsulfur pentafluoride (MANCHESTER, 0.042 g, 0.192 mmol) was added and the mixture was stirred under reflux overnight. Solvent was removed in vacuo and the crude mixture was purified by preparative HPLC (SunFire 19×150 mm, H2O 0.1% TFA-ACN 0.1% TFA gradient from 10 to 100%) to yield the title compound as a beige solid.

후처리

  1. additionwas added
  2. temperatureunder reflux overnight
  3. customSolvent was removed in vacuo
  4. customthe crude mixture was purified by preparative HPLC (SunFire 19×150 mm, H2O 0.1% TFA-ACN 0.1% TFA gradient from 10 to 100%)

출처 및 근거

ORD 기록
ord-a1603277a1ae49b2b9f61a4b92f3a6fc
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238653B2

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