Hydrochloric Acid → HCID 178522413, 화합물

HRID 529740노트

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HRID 529740 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:33][CH:34]([F:36])[F:35])=[C:6]([C:8]2[N:12](COCC[Si](C)(C)C)[N:11]=[CH:10][C:9]=2[NH:21][C:22]([C:24]2[CH:25]=[N:26][N:27]3[CH:32]=[CH:31][CH:30]=[N:29][C:28]=23)=[O:23])[CH:7]=1.Cl>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:33][CH:34]([F:36])[F:35])=[C:6]([C:8]2[C:9]([NH:21][C:22]([C:24]3[CH:25]=[N:26][N:27]4[CH:32]=[CH:31][CH:30]=[N:29][C:28]=34)=[O:23])=[CH:10][NH:11][N:12]=2)[CH:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 131735618pyrazolo[1,5-a]pyrimidine-3-carboxylic acid [5-(5-chloro-2-difluoromethoxyphenyl)-1-(2-trimethylsilanylethoxymethyl)-1H-pyrazol-4-yl]amide

생성물 1

HCID 178522413HCID 178522413, 화합물수율 96.4%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

A suspension of pyrazolo[1,5-a]pyrimidine-3-carboxylic acid [5-(5-chloro-2-difluoromethoxyphenyl)-1-(2-trimethylsilanylethoxymethyl)-1H-pyrazol-4-yl]amide (59.0 g, 110 mmol) in methanol (420 mL) was treated with 6N HCl (80 mL) and the mixture heated at 60° C. for 4 hours. The solvent was evaporated and the residue triturated with water. The solid was collected by filtration, washed with water and left to air dry. The solid was triturated with a minimum volume of acetonitrile, collected by filtration, washed with diethyl ether and dried at 60° C. under high vacuum to afford the title compound as a yellow solid (42.9 g, 96%). 1H NMR (400 MHz, DMSO-d6) δ: (ppm) 9.71 (s, 1H), 9.34 (dd, 1H), 8.68-8.69 (m, 1H), 8.66 (s, 1H), 8.25 (s, 1H), 7.62 (dd, 2H), 7.43-7.46 (m, 1H), 7.29 (dd, 1H), 7.23 (d, 1H).

후처리

  1. customThe solvent was evaporated
  2. customthe residue triturated with water
  3. filtrationThe solid was collected by filtration
  4. washwashed with water
  5. waitleft to air
  6. customdry
  7. customThe solid was triturated with a minimum volume of acetonitrile
  8. filtrationcollected by filtration
  9. washwashed with diethyl ether
  10. customdried at 60° C. under high vacuum

출처 및 근거

ORD 기록
ord-8bfd11f024e34e59bf34321fac942dd0
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346815B2

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