Sodium hydride → HCID 86662320、化合物

HRID 449643ノート

反応式

HRID 449643 の反応式
[CH3:1][N:2]([CH3:8])[CH2:3][C:4]([CH3:7])([OH:6])[CH3:5].[Br:9][C:10]1[N:11]=[N:12][C:13](Br)=[CH:14][CH:15]=1.[H-].[Na+]>C1COCC1>[Br:9][C:10]1[N:11]=[N:12][C:13]([O:6][C:4]([CH3:7])([CH3:5])[CH2:3][N:2]([CH3:8])[CH3:1])=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 2488523,6-DibromopyridazineHCID 97937381-(Dimethylamino)-2-methylpropan-2-ol

生成物 1

HCID 86662320HCID 86662320、化合物収率 65.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

In a 100 mL round bottom flask was added 1-(dimethylamino)-2-methylpropan-2-ol (1.48 g, 12.6 mmol, Eq: 1.5), THF and 3,6-dibromopyridazine (2 g, 8.41 mmol, Eq: 1.00). The flask was cooled to 0° C. followed by addition of NaH (572 mg, 14.3 mmol, Eq: 1.7) in one portion. The turbid reaction mixture was allowed to warm to room temperature and was stirred at room temperature overnight. The resultant black reaction mixture was absorbed onto silica gel and purified by LC chromatography eluting with 0-5% MeOH in 1/1 EtOAc/Hex to afford 1.5 g (65%) of the title compound.

後処理

  1. customThe turbid reaction mixture
  2. temperatureto warm to room temperature
  3. customThe resultant black reaction mixture
  4. customwas absorbed onto silica gel
  5. custompurified by LC chromatography
  6. washeluting with 0-5% MeOH in 1/1 EtOAc/Hex

出典と根拠

ORDレコード
ord-40e996f4ac5b45199b6b38b6571d5db8
出典データセット
uspto-grants-2013_07
特許番号
US08481540B2

反応ノート

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