Sodium Nitrite → HCID 178494309, 화합물

HRID 1487982노트

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HRID 1487982 반응식
[CH:1]1([C:5]2[C:13]([C:14]3[NH:18][C:17]([O:19][CH3:20])=[N:16][N:15]=3)=[CH:12][C:8]([C:9](N)=[O:10])=[C:7]([CH3:21])[CH:6]=2)[CH2:4][CH2:3][CH2:2]1.N([O-])=[O:23].[Na+]>C(O)(C(F)(F)F)=O>[CH:1]1([C:5]2[C:13]([C:14]3[NH:18][C:17]([O:19][CH3:20])=[N:16][N:15]=3)=[CH:12][C:8]([C:9]([OH:23])=[O:10])=[C:7]([CH3:21])[CH:6]=2)[CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 23668193Sodium NitriteHCID 178494303HCID 178494303, 화합물2회

생성물 1

HCID 178494309HCID 178494309, 화합물

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

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온도
0 °C

실험 절차

To a solution of 4-cyclobutyl-5-(5-methoxy-4H-1,2,4-triazol-3-yl)-2-methylbenzamide (compound 89.8, 0.1 g, 0.33 mmol) in TFA (5 mL) at 0° C., was added NaNO2 (46 mg, 0.66 mmol). The mixture was stirred at 0° C. for 1 hour, then at room temperature for 2 hours. The mixture was concentrated under reduced pressure and the residue was partitioned between EtOAc and brine. The aqueous layer was extracted with EtOAc and the combined organic layers were dried (Na2SO4), filtered and concentrated under reduced pressure to yield 0.1 g (theoretical) of the title compound as a clear oil. m/z (ES+) 288 (M+H)+.

후처리

  1. waitat room temperature for 2 hours
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customthe residue was partitioned between EtOAc and brine
  4. extractionThe aqueous layer was extracted with EtOAc
  5. dry with materialthe combined organic layers were dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d43a31c1171d4774a6f376d63411d822
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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