Dimethylformamide → HCID 66767080、化合物

HRID 2195506ノート

反応式

HRID 2195506 の反応式
[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]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 1230531,2-Difluoro-4-nitrobenzeneHCID 516892Sodium BicarbonateHCID 66766901HCID 66766901、化合物

生成物 1

HCID 66767080HCID 66767080、化合物収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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.

出典と根拠

ORDレコード
ord-e9bad44593d246de84a4977cf428ddd7
出典データセット
uspto-grants-2012_12
特許番号
USRE043878E1

反応ノート

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