Hydrochloric Acid → HCID 11955840, 화합물

HRID 600774

반응식

HRID 600774 반응식
C([O:3][C:4]1[CH2:13][C:12]2[C:11]([NH:14][C:15]3[O:16][C:17]([C:20]4[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=4)=[CH:18][N:19]=3)=[CH:10][CH:9]=[CH:8][C:7]=2[CH2:6][CH:5]=1)C.Cl.C([O-])(O)=O.[Na+]>O1CCCC1>[F:29][C:26]([F:27])([F:28])[C:23]1[CH:24]=[CH:25][C:20]([C:17]2[O:16][C:15]([NH:14][C:11]3[CH:10]=[CH:9][CH:8]=[C:7]4[C:12]=3[CH2:13][C:4](=[O:3])[CH2:5][CH2:6]4)=[N:19][CH:18]=2)=[CH:21][CH:22]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 67229299N-(7-ethoxy-5,8-dihydronaphthalen-1-yl)-5-[4-(trifluoromethyl)phenyl]-1,3-oxazol-2-amine

생성물 1

HCID 11955840HCID 11955840, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

A solution of the product of Example 1H (150 mg, 0.375 mmol) in tetrahydrofuran (2.3 mL) was treated with 2N HCl (0.76 mL, 1.52 mmol), and the mixture was heated at 40° C. for 1 hour. After cooling to room temperature, the solution was brought to pH 8 with saturated NaHCO3 solution, and extracted with ethyl acetate. The organic extracts were washed with H2O, dried over Na2SO4, filtered and evaporated in vacuo to the title compound as a brown residue (140 mg, 100%). 1H NMR (DMSO-d6) δ 9.56 (s, 1H), 7.78 (m, 4H), 7.67 (d, 1H, J=7.8 Hz), 7.62 (s, 1H), 7.22 (t, 1H, J=7.8 Hz), 7.06 (d, 1H, J=7.4 Hz), 3.58 (s, 2H), 3.36 (m, 2H), 3.06 (t, 2H, J=6.8 Hz); MS (ESI+) m/z 373 (M+H)+.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic extracts were washed with H2O
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated in vacuo to the title compound as a brown residue (140 mg, 100%)

출처 및 근거

ORD 기록
ord-881d0d0f502e4173bb6141fbfdb8aff9
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902236B2

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