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

HRID 549240노트

반응식

HRID 549240 반응식
C([O-])(=O)C.[K+].[Br:6]Br.[CH2:8]([N:11]1[C:15]([CH2:16][CH:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)=[CH:14][C:13]([C:23]#[N:24])=[N:12]1)[CH2:9][CH3:10].S([O-])(O)=O.[Na+]>C(O)(=O)C>[Br:6][C:14]1[C:13]([C:23]#[N:24])=[N:12][N:11]([CH2:8][CH2:9][CH3:10])[C:15]=1[CH2:16][CH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1

참가 물질

6

반응물 4

HCID 24408BromineHCID 517044Potassium AcetateHCID 23665763Sodium BisulfiteHCID 671577501-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile

생성물 1

HCID 671583524-bromo-1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile수율 98.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Potassium acetate (3.93 g, 40.0 mmol) and bromine (3.58 g, 22.4 mmol) were sequentially added to a solution of 1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile (3.98 g, 16 mmol) in acetic acid (32 mL). The reaction was stirred for 40 hours at room temperature. Saturated aqueous sodium hydrogensulfite was added until the reaction became colorless. Most of the acetic acid was removed under reduced pressure, and 2M aqueous sodium carbonate was added. A precipitate formed, was isolated by filtration, washed with water, and dried on the vacuum filter funnel to provide 4.91 g of 4-bromo-1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile as a white solid.

후처리

  1. customMost of the acetic acid was removed under reduced pressure, and 2M aqueous sodium carbonate
  2. additionwas added
  3. customA precipitate formed
  4. customwas isolated by filtration
  5. washwashed with water
  6. customdried on the vacuum
  7. filtrationfilter funnel

출처 및 근거

ORD 기록
ord-71e8c9ddfafa4b6f9a91d5c5248c46c7
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943636B2

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