Hydrazine hydrate (1:1) → Ethyl 4-{6-[1-(acetylamino)propyl]-5-oxo-4,5-dihydro-1,2,4-triazin-3-yl}benzoate

HRID 1791182노트

반응식

HRID 1791182 반응식
Cl.[NH2:2][C:3](=[NH:15])[C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1.O.[NH2:17]N.[C:19]([NH:22][CH:23]([CH2:31][CH3:32])[C:24](=O)[C:25](OCC)=[O:26])(=[O:21])[CH3:20]>C(O)C>[C:19]([NH:22][CH:23]([C:24]1[C:25](=[O:26])[NH:15][C:3]([C:4]2[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=2)=[N:2][N:17]=1)[CH2:31][CH3:32])(=[O:21])[CH3:20]

참가 물질

5

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 12710118Benzoic acid, 4-(aminoiminomethyl)-, ethyl ester, hydrochloride (1:1)HCID 21935058Ethyl 3-acetamido-2-oxopentanoate

생성물 1

HCID 135682026Ethyl 4-{6-[1-(acetylamino)propyl]-5-oxo-4,5-dihydro-1,2,4-triazin-3-yl}benzoate

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

1.98 g (8.66 mmol) ethyl 4-[amino(imino)methyl]benzoate hydrochloride are suspended in 50 ml of ethanol and 1.47 g (10.2 mmol, 1.2 equiv.) hydrazine hydrate are added. After stirring at room temperature for 1 hour, 2.59 g (13 mmol, 1.5 equiv.) of the compound of Example 2A, dissolved in 10 ml of ethanol, are added. The reaction mixture is stirred at 80° C. (bath temperature) for 4 hours and then at room temperature over night. The mixture is evaporated to dryness in vacuo and the product is purified by chromatography (flash or column chromatography or preparative HPLC).

후처리

  1. additionare added
  2. stirringThe reaction mixture is stirred at 80° C. (bath temperature) for 4 hours
  3. waitat room temperature over night
  4. customThe mixture is evaporated to dryness in vacuo
  5. customthe product is purified by chromatography (flash or column chromatography or preparative HPLC)

출처 및 근거

ORD 기록
ord-1e2a99234f7f4c078ff0b3dc5a472c6e
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07074790B2

반응 노트

불러오는 중…