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

HRID 549245노트

반응식

HRID 549245 반응식
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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-b31a214119004e15a1b30be08ad3338e
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943636B2

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