Acetic Acid → 2-Bromo-3-(but-2-ynyl)-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one

HRID 350663노트

반응식

HRID 350663 반응식
O.[NH2:2][NH2:3].[Br:4][C:5]1[N:9]([CH2:10][C:11]#[C:12][CH3:13])[C:8]([C:14]([O:16]C)=O)=[C:7]([CH:18]=O)[N:6]=1.C(O)(=O)C>C(O)C>[Br:4][C:5]1[N:9]([CH2:10][C:11]#[C:12][CH3:13])[C:8]2[C:14](=[O:16])[NH:3][N:2]=[CH:18][C:7]=2[N:6]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 21947682methyl 2-bromo-3-(2-butyn-1-yl)-5-formyl-3H-imidazole-4-carboxylate

생성물 1

HCID 219476582-Bromo-3-(but-2-ynyl)-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

0.31 ml of hydrazine hydrate (99%), dissolved in 1 ml of ethanol, are added dropwise at ambient temperature to a solution of 1.80 g of methyl 2-bromo-3-(2-butyn-1-yl)-5-formyl-3H-imidazole-4-carboxylate in 25 ml of ethanol. Five minutes later 1.5 ml of concentrated acetic acid are added and the mixture is refluxed for 30 minutes. After cooling the precipitated solid is suction filtered, washed with 10 ml of ethanol and 20 ml of diethyl ether and dried.

후처리

  1. temperaturethe mixture is refluxed for 30 minutes
  2. temperatureAfter cooling the precipitated solid
  3. filtrationfiltered
  4. washwashed with 10 ml of ethanol and 20 ml of diethyl ether
  5. customdried

출처 및 근거

ORD 기록
ord-69a4d8058cb64f0cb04c9d95639208a8
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183280B2

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