HRID590834

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID78373

Methanamine, 1,1-dimethoxy-N,N-dimethyl-

C5H13NO2

结构：Cc1nc(Cl)cc2c1c(I)nn2C(c1ccccc1)(c1ccccc1)c1ccccc1

HCID118168962

未命名化合物

2 次

PRODUCTS

生成物

HCID138539

Cyclopentyl methyl ether

C6H12O

结构：CN(C)/C=C/c1nc(Cl)cc2c1c(I)nn2C(c1ccccc1)(c1ccccc1)c1ccccc1

HCID118272432

未命名化合物

PROCEDURE

实验过程

6-chloro-3-iodo-trityl-1H-pyrazolo[4.3-c]pyridine (Intermediate 1C, 2 g, 3.73 mmol), N, N-dimethylformamide-dimethyl acetal (DMF-DMA) (4.45 g, 37.3 mmol) were stirred at 125° C. for 12 hrs. Reaction was concentrated and excess DMF-DMA azeotroped with toluene. Trituration with cylopentylmethylether gave (E)-2-(6-chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)-N,N-dimethylethenamine. MS ESI calc'd. for C29H24ClIN4 [M+H]+ 591. found 591.

WORKUP

后处理

customReaction
concentrationwas concentrated
customexcess DMF-DMA azeotroped with toluene

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-8cc57f8246b24be5a48b78a85e7c3156
来源数据集: uspto-grants-2016_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09233979B2
来源说明: uspto-grants-2016_01

反应 SMILES

[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]2[C:9]([I:31])=[N:10][N:11]([C:12]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:4]=2[CH:3]=1.[CH3:32][O:33][CH:34](OC)[N:35]([CH3:37])[CH3:36]>>[CH:25]1([O:33][CH3:32])[CH2:30][CH2:29][CH2:28][CH2:27]1.[Cl:1][C:2]1[N:7]=[C:6](/[CH:8]=[CH:34]/[N:35]([CH3:37])[CH3:36])[C:5]2[C:9]([I:31])=[N:10][N:11]([C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)[C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:4]=2[CH:3]=1