1-Hydroxybenzotriazole → HCID 45810073、化合物

HRID 1038004

反応式

HRID 1038004 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][N:8]=[C:7]2[C:13]([OH:15])=O)([O-:3])=[O:2].Cl.CN.C1C=CC2N(O)N=[N:25][C:23]=2C=1.CCN(C(C)C)C(C)C.Cl.CN(C)CCCN=C=NCC>CN1CCCC1=O.C(OCC)(=O)C>[CH3:23][NH:25][C:13]([C:7]1[C:6]2[C:10](=[CH:11][CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[NH:9][N:8]=1)=[O:15]

参加物

8

反応物 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 6364545Methylamine hydrochlorideHCID 71446525-nitro-1H-indazole-3-carboxylic Acid

生成物 1

HCID 45810073HCID 45810073、化合物収率 63%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

To a solution of compound 54 (100 mg, 0.483 mmol), methylamine hydrochloride (52.2 mg, 0.773 mmol), HOBt (130 mg, 0.966 mmol) and DIEA (0.34 mL, 1.95 mmol) in N-methylpyrrolidinone was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (148 mg, 0.773 mmol). The reaction was stirred at room temperature for 2 hrs and diluted with 10 mL of ethyl acetate. The mixture was washed with water and a yellow solid precipitated. The precipitate was collected by filtration to give compound 55 (67 mg).

後処理

  1. washThe mixture was washed with water
  2. customa yellow solid precipitated
  3. filtrationThe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-335486c23e0a485da576a6cc9d5265b4
出典データセット
uspto-grants-2013_10
特許番号
US08546404B2

関連ノート

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