Water → HCID 67326247、化合物

HRID 2199313ノート

反応式

HRID 2199313 の反応式
[CH3:1][C:2]1[CH:12]=[CH:11][C:10]([NH:13][C:14](=[O:33])[C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]3[CH2:27][CH2:26][N:25]([CH3:28])[CH2:24][CH2:23]3)=[C:17]([C:29]([F:32])([F:31])[F:30])[CH:16]=2)=[CH:9][C:3]=1[C:4](OCC)=[O:5].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[O-]S([O-])(=O)=O.[Mg+2]>C1COCC1.C(OCC)C>[OH:5][CH2:4][C:3]1[CH:9]=[C:10]([NH:13][C:14](=[O:33])[C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]3[CH2:23][CH2:24][N:25]([CH3:28])[CH2:26][CH2:27]3)=[C:17]([C:29]([F:32])([F:30])[F:31])[CH:16]=2)[CH:11]=[CH:12][C:2]=1[CH3:1]

参加物

7

反応物 4

HCID 962WaterHCID 24083Sulfuric acid magnesium salt (1:1)HCID 21226445Aluminium lithium hydrideHCID 67347178HCID 67347178、化合物

生成物 1

HCID 67326247HCID 67326247、化合物収率 84%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution Ethyl 2-methyl-5-(4-((4-methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)benzamido)benzoate (300 mg, 0.65 mmol) in dried THF (2.2 mL) was added Lithium aluminium hydride 2.0M THF solution (0.48 mL, 0.98 mmol) at 0° C. The reaction mixture was stirred for 2 hours at room temperature. When the reaction was completed, the reaction mixture was diluted with ethyl ether (2.0 mL) and added water very slowly to decompose the excess of the reagent. To a reaction mixture was added MgSO4, celite filtered and concentrated under reduced pressure. The title compound (230 mg, 84% yield) was used next step without further purification. MS m/z: 422 [M+1].

後処理

  1. filtrationfiltered
  2. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ac3fff0521a449d9b2b8851618c4571a
出典データセット
uspto-grants-2016_06
特許番号
US09358231B2

反応ノート

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