Hydrochloric Acid → HCID 59201113, 화합물

HRID 1690161

반응식

HRID 1690161 반응식
[F:1][C:2]([F:23])([F:22])[C:3]([C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[C:14]([CH2:19][CH2:20][CH3:21])[CH:13]=1)([O:8][CH2:9][O:10][CH3:11])[C:4]([F:7])([F:6])[F:5].C(=O)([O-])[O-].[K+].[K+].Cl[C:31]1[CH:32]=[C:33]([C:38]([N+:41]([O-:43])=[O:42])=[CH:39][N:40]=1)[C:34]([O:36][CH3:37])=[O:35].Cl>CN(C)C=O.O>[F:1][C:2]([F:22])([F:23])[C:3]([C:12]1[CH:17]=[CH:16][C:15]([O:18][C:31]2[CH:32]=[C:33]([C:38]([N+:41]([O-:43])=[O:42])=[CH:39][N:40]=2)[C:34]([O:36][CH3:37])=[O:35])=[C:14]([CH2:19][CH2:20][CH3:21])[CH:13]=1)([O:8][CH2:9][O:10][CH3:11])[C:4]([F:6])([F:5])[F:7]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 45480451Methyl 2-chloro-5-nitroisonicotinateHCID 59201037HCID 59201037, 화합물

생성물 1

HCID 59201113HCID 59201113, 화합물수율 73%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-(1,1,1,3,3,3-hexafluoro-2-(methoxymethoxy)propan-2-yl)-2-propylphenol (1.68 g, 4.86 mmol) in N,N-dimethylformamide (30 mL), potassium carbonate (1.34 g) and methyl 2-chloro-5-nitroisonicotinate (1.58 g) were added, and the resultant mixture was stirred in an oil bath with the oil temperature at 80° C. After completion of the reaction, the reaction solution was neutralized by adding 2 mol/L of hydrochloric acid, added with water, and extracted with ethyl acetate. Subsequently, the organic layer was washed with brine, dried using anhydrous sodium sulfate, and concentrated in vacuo. The residue was purified using thin-layer silica-gel column chromatography (hexane/ethyl acetate) and the title compound (1.86 g, yield 73%) was obtained as a colorless oil.

후처리

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. washSubsequently, the organic layer was washed with brine
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified

출처 및 근거

ORD 기록
ord-bcc702a03ad14fe68fb779b91f86e0a3
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08153634B2

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