Hydrochloric Acid → 4-[6-(Difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylic acid

HRID 1842607노트

반응식

HRID 1842607 반응식
C[O:2][C:3]([C:5]1[S:6][C:7]([CH3:23])=[C:8]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[C:17]([O:19][CH:20]([F:22])[F:21])[CH:16]=[N:15][C:14]=23)[CH:9]=1)=[O:4].[OH-].[K+].CO.Cl>C1COCC1>[F:22][CH:20]([F:21])[O:19][C:17]1[CH:16]=[N:15][C:14]2[N:13]([N:12]=[CH:11][C:10]=2[C:8]2[CH:9]=[C:5]([C:3]([OH:4])=[O:2])[S:6][C:7]=2[CH3:23])[CH:18]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14797Potassium HydroxideHCID 68304950Methyl-4-[6-(difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylate

생성물 1

HCID 683051734-[6-(Difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylic acid수율 64.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

Methyl-4-[6-(difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylate (0.916 g, 2.70 mmol) was dissolved in THF (4 mL). 1 M KOH in MeOH (12.0 mL, 12.0 mmol) was added and the reaction heated to 40° C. for 16 h. After the hydrolysis was complete, treated with 1N HCl and the resulting solids were filtered, washed with water and dried to afford the title compound (0.568 g, 1.75 mmol). LRMS (APCI) calc'd for (C13H9F2N3O3S) [M+H]+, 326.0; found 326.0.

후처리

  1. filtrationthe resulting solids were filtered
  2. washwashed with water
  3. customdried

출처 및 근거

ORD 기록
ord-1e437e41b5dd443d90caf748b8be3afa
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946237B2

반응 노트

불러오는 중…