Triethylamine → HCID 68840826、化合物

HRID 229729

反応式

HRID 229729 の反応式
[CH3:1][CH:2]1[CH2:11][C:10]2[NH:9][N:8]=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)[CH2:6][C:5]=2[C:4](=O)[CH2:3]1.Cl.[NH2:24][NH2:25].C(N(CC)CC)C>C(O)C>[CH3:1][CH:2]1[CH2:11][C:10]2[N:9]=[N:8][C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)=[CH:6][C:5]=2[C:4](=[N:24][NH2:25])[CH2:3]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 115031Hydrazinium chlorideHCID 42467327-Methyl-3-(3-(trifluoromethyl)phenyl)-1,4,6,7,8-pentahydrocinnolin-5-one

生成物 1

HCID 68840826HCID 68840826、化合物収率 12.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To an ethanol solution (3 mL) of 7-methyl-3-(3-trifluoromethylphenyl)-4,6,7,8-terahydro-1H-cinnolin-5-one (230 mg, 0.74 mmol) obtained in Example 65 were added hydrazine hydrochloride (77.3 mg, 0.74 mmol) and triethylamine (0.206 mL, 1.48 mmol) and stirred at room temperature over night. The reaction liquid was concentrated, followed by purification of residue with silica gel column chromatography (hexane/ethyl acetate=1/1) to obtain an objective compound (29.5 mg, 12.5%).

後処理

  1. customThe reaction liquid
  2. concentrationwas concentrated
  3. customfollowed by purification of residue with silica gel column chromatography (hexane/ethyl acetate=1/1)

出典と根拠

ORDレコード
ord-392929630b374aabaa55e4ad9670f4d9
出典データセット
uspto-grants-2009_07
特許番号
US07563893B2

関連ノート

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