Ammonium Hydroxide → 1-butyl-5-methyl-1H-pyrazole-3-carboxamide

HRID 1360407노트

반응식

HRID 1360407 반응식
[CH2:1]([N:5]1[C:9]([CH3:10])=[CH:8][C:7]([C:11]([O:13]CC)=O)=[N:6]1)[CH2:2][CH2:3][CH3:4].[OH-].[NH4+:17]>CO>[CH2:1]([N:5]1[C:9]([CH3:10])=[CH:8][C:7]([C:11]([NH2:17])=[O:13])=[N:6]1)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 66958271ethyl 1-butyl-5-methyl-1H-pyrazole-3-carboxylate

생성물 1

HCID 669589581-butyl-5-methyl-1H-pyrazole-3-carboxamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of ethyl 1-butyl-5-methyl-1H-pyrazole-3-carboxylate (18.1 g, 86.1 mmol) in methanol (25 mL) was treated with ammonium hydroxide (25 mL) according to a modification of the method described in Part D of Examples 1-4. At the end of the reaction, the methanol was removed under reduced pressure, and the remaining solution was cooled in a refrigerator. A precipitate formed, was isolated by filtration, and was washed with water. The solid (9 g) was recrystallized from hexane (300 mL) and ethyl acetate (30 mL), isolated by filtration, washed with hexane, and air-dried to provide 6.95 g of 1-butyl-5-methyl-1H-pyrazole-3-carboxamide as colorless plates, mp 113.5-114.5° C.

후처리

  1. customAt the end of the reaction
  2. customthe methanol was removed under reduced pressure
  3. temperaturethe remaining solution was cooled in a refrigerator
  4. customA precipitate formed
  5. customwas isolated by filtration
  6. washwas washed with water
  7. customThe solid (9 g) was recrystallized from hexane (300 mL) and ethyl acetate (30 mL)
  8. customisolated by filtration
  9. washwashed with hexane
  10. customair-dried

출처 및 근거

ORD 기록
ord-5065ce42aaab450d84aa5c6470bb1b81
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07879849B2

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