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

HRID 1791182ノート

反応式

HRID 1791182 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-1e2a99234f7f4c078ff0b3dc5a472c6e
出典データセット
uspto-grants-2006_07
特許番号
US07074790B2

反応ノート

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