HRID1049499

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID13831

Tributylphosphine

C12H27P

HCID73042

1,1′-(1,2-Diazenediyl)bis[1-(1-piperidinyl)methanone]

C12H20N4O2

HCID117759635

未命名化合物

HCID178491816

未命名化合物

PRODUCTS

生成物

结构：CCOC(=O)CC(c1cc(COc2ccc(-c3cc(OC)ccc3F)c(CC(C)(C)C)n2)ncn1)C1CC1

HCID117759676

未命名化合物

收率 64.6%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

Under a nitrogen atmosphere, to a solution of 5-(2-fluoro-5-methoxyphenyl)-6-neopentylpyridin-2-ol (200 mg) and ethyl 3-cyclopropyl-3-(6-(hydroxymethyl)pyrimidin-4-yl)propanoate (173 mg) in THF (5.0 mL) were added 1,1′-(azodicarbonyl)dipiperidine (279 mg) and tributylphosphine (273 μL) at room temperature, and the mixture was stirred for 4 hr. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (233 mg) as a colorless oil.

WORKUP

后处理

customThe solvent was evaporated under reduced pressure
customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-611a4f79d47c4359b8d89d6203a69e87
来源数据集: uspto-grants-2016_07
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09382188B2
来源说明: uspto-grants-2016_07

反应 SMILES

[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:11]=[CH:12][C:13]([OH:21])=[N:14][C:15]=1[CH2:16][C:17]([CH3:20])([CH3:19])[CH3:18].[CH:22]1([CH:25]([C:32]2[CH:37]=[C:36]([CH2:38]O)[N:35]=[CH:34][N:33]=2)[CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:24][CH2:23]1.N(C(N1CCCCC1)=O)=NC(N1CCCCC1)=O.C(P(CCCC)CCCC)CCC>C1COCC1>[CH:22]1([CH:25]([C:32]2[CH:37]=[C:36]([CH2:38][O:21][C:13]3[CH:12]=[CH:11][C:10]([C:3]4[CH:4]=[C:5]([O:8][CH3:9])[CH:6]=[CH:7][C:2]=4[F:1])=[C:15]([CH2:16][C:17]([CH3:18])([CH3:20])[CH3:19])[N:14]=3)[N:35]=[CH:34][N:33]=2)[CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:24][CH2:23]1