HRID1011231

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID81531

Diisopropylethylamine

C8H19N

结构：O=C(NCc1ccc(Cl)cc1Cl)c1cn(C2CC2)c2c(Cl)c(F)c(F)cc2c1=O

HCID57780978

未命名化合物

HCID60145982

2,8-Diazaspiro[4.5]decan-3-one--hydrogen chloride (1/1)

C8H15ClN2O

PRODUCTS

生成物

结构：O=C1CC2(CCN(c3c(F)cc4c(=O)c(C(=O)NCc5ccc(Cl)cc5Cl)cn(C5CC5)c4c3Cl)CC2)CN1

HCID57780959

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID679

Dimethyl sulfoxide

C2H6OS

PROCEDURE

实验过程

60 mg (0.13 mmol) of the compound of Example 70A and 37 mg (0.20 mmol) of 3-oxo-2,8-diazaspiro[4,5]decane hydrochloride (Example 13A) are stirred with 91 μl (0.52 mmol) of N,N-diisopropylethylamine in 2 ml of DMSO at 120° C. for 2 days. After cooling, the entire reaction mixture is separated by preparative HPLC (method 5). Concentration of the appropriate fractions on a rotary evaporator and drying under high vacuum give 20 mg (26% of theory) of the title compound.

WORKUP

后处理

temperatureAfter cooling
customthe entire reaction mixture
customis separated by preparative HPLC (method 5)
customConcentration of the appropriate fractions on a rotary evaporator
customdrying under high vacuum

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-8f67c244a1c441eeb4cdc5f5d55a5849
来源数据集: uspto-grants-2011_07
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07977349B2
来源说明: uspto-grants-2011_07

反应 SMILES

[Cl:1][C:2]1[C:3](F)=[C:4]([F:28])[CH:5]=[C:6]2[C:11]=1[N:10]([CH:12]1[CH2:14][CH2:13]1)[CH:9]=[C:8]([C:15]([NH:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=1[Cl:26])=[O:16])[C:7]2=[O:27].Cl.[O:31]=[C:32]1[CH2:36][C:35]2([CH2:41][CH2:40][NH:39][CH2:38][CH2:37]2)[CH2:34][NH:33]1.C(N(CC)C(C)C)(C)C>CS(C)=O>[Cl:1][C:2]1[C:3]([N:39]2[CH2:38][CH2:37][C:35]3([CH2:34][NH:33][C:32](=[O:31])[CH2:36]3)[CH2:41][CH2:40]2)=[C:4]([F:28])[CH:5]=[C:6]2[C:11]=1[N:10]([CH:12]1[CH2:14][CH2:13]1)[CH:9]=[C:8]([C:15]([NH:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=1[Cl:26])=[O:16])[C:7]2=[O:27]