Water → HCID 69300599、化合物

HRID 2196531ノート

反応式

HRID 2196531 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:10]([C:11]2[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=2)[C:14]#[N:15])[N:9]=[C:8]([C:19]([F:22])([F:21])[F:20])[CH:7]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:10]([C:11]2[CH:12]=[C:13]([CH2:14][NH2:15])[CH:16]=[CH:17][CH:18]=2)[N:9]=[C:8]([C:19]([F:21])([F:20])[F:22])[CH:7]=1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 158809863-[3-(Trifluoromethyl)-5-(2-furanyl)-1H-pyrazole-1-yl]benzonitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 69300599HCID 69300599、化合物収率 100%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 53 (3 g, 9.89 mmol) in THF (50 mL) at 0° C. was added lithium aluminium hydride (0.939 g, 24.73 mmol). The resulting suspension was allowed to stir for 0.5 h. The reaction mixture was then warmed to room temperature and stirred for another 1 h. The following was added sequentially: 0.9 mL of water, 0.9 mL of 15% NaOH and 1.8 mL of water. The white solid was removed by filtration and the filtrate evaporated under vacuum. The title product 54 (3.04 g, 100% yield) was isolated as a pale yellow oil. Crude was used without any further purification. LRMS (ESI): calc. 307.3; found 308.4 (MH)+.

後処理

  1. stirringstirred for another 1 h
  2. additionThe following was added sequentially
  3. customThe white solid was removed by filtration
  4. customthe filtrate evaporated under vacuum

出典と根拠

ORDレコード
ord-7c3ac86c7c5f4d36a3db2df3297dfda9
出典データセット
uspto-grants-2012_12
特許番号
US08338437B2

反応ノート

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