Sodium Nitrite → HCID 178467500, 화합물

HRID 541362노트

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HRID 541362 반응식
[CH:1]1([C:5]2[C:13]([C:14]3[NH:18][C:17]([O:19][CH2:20][CH3:21])=[N:16][N:15]=3)=[CH:12][C:8]([C:9](N)=[O:10])=[C:7]([CH3:22])[CH:6]=2)[CH2:4][CH2:3][CH2:2]1.N([O-])=[O:24].[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][CH2:20][CH3:21])=[N:16][N:15]=3)=[CH:12][C:8]([C:9]([OH:24])=[O:10])=[C:7]([CH3:22])[CH:6]=2)[CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 23668193Sodium NitriteHCID 178467490HCID 178467490, 화합물

생성물 1

HCID 178467500HCID 178467500, 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-ethoxy-4H-1,2,4-triazol-3-yl)-2-methylbenzamide (219.8, 0.1 g, 0.33 mmol) in TFA (5 ml) was added NaNO2 (0.046 g, 0.66 mmol) at 0° C. The mixture was stirred at 0° C. for 1 hour then at room temperature for 2 hours. The mixture was concentrated under reduced pressure. The residue was partitioned between EtOAc and brine. The aqueous layer was extracted with EtOAc. The combined organic layers were dried (Na2SO4) and concentrated to give a clear oil. Yield: 0.1 g, 100%. m/z (ES−) 300 (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. concentrationconcentrated
  7. customto give a clear oil

출처 및 근거

ORD 기록
ord-6b172f2c2c694d15b176d4bfd8310c24
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871790B2

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