Dimethylformamide → HCID 66767080, 화합물

HRID 2195506노트

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HRID 2195506 반응식
[OH:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:7]([CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][O:17]1)[N:6]=[CH:5]2.F[C:23]1[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][C:24]=1[F:32].C([O-])(O)=O.[Na+].CN(C=O)C>O>[CH2:14]([O:13][C:11]([C:10]1[CH:9]=[C:8]2[C:4]([CH:5]=[N:6][N:7]2[CH:16]2[CH2:21][CH2:20][CH2:19][CH2:18][O:17]2)=[CH:3][C:2]=1[O:1][C:23]1[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][C:24]=1[F:32])=[O:12])[CH3:15]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 1230531,2-Difluoro-4-nitrobenzeneHCID 516892Sodium BicarbonateHCID 66766901HCID 66766901, 화합물

생성물 1

HCID 66767080HCID 66767080, 화합물수율 95%

시약·촉매·용매 1

HCID 962Water용매

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온도
80 °C

실험 절차

A mixture of ethyl 5-hydroxy-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole-6-carboxylate (10.8 g, 37 mmol), 1,2-difluoro-4-nitrobenzene (7.1 g, 44 mmol), NaHCO3 (7.4 g, 88 mmol) and DMF (100 mL) is stirred at 80° C. for 2 hours. After it is cooled to RT, water (400 mL) and PE (50 mL) are added and the mixture is stirred for 20 min. The precipitate is collected and dried under vacuum at 50° C. to afford the product (15 g, 95% yield). MS (m/z): 430.1 (M+H).

후처리

  1. temperatureAfter it is cooled to RT
  2. stirringthe mixture is stirred for 20 min
  3. customThe precipitate is collected
  4. customdried under vacuum at 50° C.

출처 및 근거

ORD 기록
ord-e9bad44593d246de84a4977cf428ddd7
출처 데이터셋
uspto-grants-2012_12
특허 번호
USRE043878E1

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