Bromine → 4-bromo-1-(2-methoxyethyl)-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile

HRID 549245ノート

反応式

HRID 549245 の反応式
C([O-])(=O)C.[K+].[Br:6]Br.[CH3:8][O:9][CH2:10][CH2:11][N:12]1[C:16]([CH2:17][CH:18]2[CH2:23][CH2:22][O:21][CH2:20][CH2:19]2)=[CH:15][C:14]([C:24]#[N:25])=[N:13]1.S([O-])(O)=O.[Na+]>C(O)(=O)C.O>[Br:6][C:15]1[C:14]([C:24]#[N:25])=[N:13][N:12]([CH2:11][CH2:10][O:9][CH3:8])[C:16]=1[CH2:17][CH:18]1[CH2:23][CH2:22][O:21][CH2:20][CH2:19]1

参加物

7

反応物 4

HCID 24408BromineHCID 517044Potassium AcetateHCID 23665763Sodium BisulfiteHCID 671574891-(2-Methoxyethyl)-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile

生成物 1

HCID 671576704-bromo-1-(2-methoxyethyl)-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile収率 90.7%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

Potassium acetate (3.12 g, 31.7 mmol) and bromine (2.84 g, 17.7 mmol) were sequentially added to a solution of 1-(2-methoxyethyl)-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile (3.16 g, 12.7 mmol) in acetic acid (25 mL). The reaction was stirred for 16 hours at room temperature. Saturated aqueous sodium hydrogensulfite was added until the reaction became colorless. Water was added, and a precipitate formed, was isolated by filtration, washed with water, and dried on the vacuum filter funnel to provide 3.78 g of 4-bromo-1-(2-methoxyethyl)-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile as a white solid containing about 2 mol % acetic acid.

後処理

  1. customa precipitate formed
  2. customwas isolated by filtration
  3. washwashed with water
  4. customdried on the vacuum
  5. filtrationfilter funnel

出典と根拠

ORDレコード
ord-b31a214119004e15a1b30be08ad3338e
出典データセット
uspto-grants-2011_05
特許番号
US07943636B2

反応ノート

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