Water → HCID 67334872, 화합물

HRID 1669841노트

반응식

HRID 1669841 반응식
C1([C:7]2[N:11]([C:12]3[CH:17]=[CH:16][C:15]([O:18][C:19]([F:22])([F:21])[F:20])=[CH:14][CH:13]=3)[N:10]=[CH:9][C:8]=2[CH2:23][C:24]2[CH:31]=[CH:30][C:27]([C:28]#N)=[CH:26][CH:25]=2)CCCCC1.[OH2:32].[OH-:33].[K+]>C(O)C>[CH2:12]1[CH2:17][CH:16]([CH:23]([C:24]2[CH:31]=[CH:30][C:27]([C:28]([OH:33])=[O:32])=[CH:26][CH:25]=2)[C:8]2[CH:9]=[N:10][N:11]([C:12]3[CH:13]=[CH:14][C:15]([O:18][C:19]([F:22])([F:20])[F:21])=[CH:16][CH:17]=3)[CH:7]=2)[CH2:15][CH2:14][CH2:13]1

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 67335137HCID 67335137, 화합물

생성물 1

HCID 67334872HCID 67334872, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a hot solution of 0.73 g 4-({5-cyclohexyl-1-[4-(trifluoromethoxy)phenyl]-1H-pyrazol-4-yl}methyl)benzonitrile From Step E above in 15 mL ethanol and 6 mL water was added 1.11 g potassium hydroxide. The resulting solution was refluxed under nitrogen over night. The solvents were removed under reduced pressure. The residue was re-suspended in 10 mL water and acidified with 9.0 mL 2 N HCl. The resulting solid was filtered, washed with water, and dried to give the title compound as a white solid. 1H NMR (CD3OD, 500 MHz) δ 7.95 (d, J=8.2 Hz, 2H), 7.48˜7.50 (m, 2H), 7.45 (d, J=8.6 Hz, 2H), 7.36 (s, 1H), 7.32 (d, J=8.2 Hz, 2H), 4.06 (s, 2H), 2.66 (tt, J=3.0 & 12.7 Hz, 1H), 1.69˜1.73 (m, 4H), 1.53˜1.64 (m, 3H), 1.09˜1.19 (m, 3H). LC-MS: 2.29 min. (M+H=445.2).

후처리

  1. temperatureThe resulting solution was refluxed under nitrogen over night
  2. customThe solvents were removed under reduced pressure
  3. filtrationThe resulting solid was filtered
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-2622226468db40eda3d4d3aa1763db79
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989475B2

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