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

HRID 591247ノート

反応式

HRID 591247 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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%)

出典と根拠

ORDレコード
ord-a1603277a1ae49b2b9f61a4b92f3a6fc
出典データセット
uspto-grants-2016_01
特許番号
US09238653B2

反応ノート

読み込み中…