1-羟基苯并三唑(HOBT) → HCID 45810073，化合物

HRID 1038004

反应方程式

HRID 1038004 反应方程式
[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]

参与物

8

反应物 5

HCID 757711-羟基苯并三唑(HOBT)HCID 81531N,N-二异丙基乙胺HCID 27239391-乙基-(3-二甲基氨基丙基)碳酰二亚胺盐酸盐HCID 6364545甲胺盐酸盐HCID 71446525-硝基吲唑-3-羧酸

产物 1

HCID 45810073HCID 45810073，化合物收率 63%

试剂、催化剂与溶剂 2

HCID 8857乙酸乙酯溶剂HCID 13387N-甲基吡咯烷酮溶剂

实验过程

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).

后处理

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

来源与证据

ORD记录
ord-335486c23e0a485da576a6cc9d5265b4
来源数据集
uspto-grants-2013_10
专利号
US08546404B2

关联笔记

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