HRID972024

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID12228

Methyl isocyanate

C2H3NO

2 次

结构：CC1(C)CC2(CC(C)(C)N1)NC(=O)N(CC(O)COc1ccc(C(C)(C)c3ccc(OCC(O)CN4C(=O)NC5(CC(C)(C)NC(C)(C)C5)C4=O)cc3)cc1)C2=O

HCID23462718

未命名化合物

PRODUCTS

生成物

结构：CNC(=O)OC(COc1ccc(C(C)(C)c2ccc(OCC(CN3C(=O)NC4(CC(C)(C)NC(C)(C)C4)C3=O)OC(=O)NC)cc2)cc1)CN1C(=O)NC2(CC(C)(C)NC(C)(C)C2)C1=O

HCID20396812

未命名化合物

PROCEDURE

实验过程

A mixture of 5.0 g of 2,2-bis{4-[2-hydroxy-3-(7,7,9,9-tetramethyl-2,4-dioxo-1,3,8-triazaspiro[4.5]dec-3-yl)propoxy]phenyl}propane (prepared as described in Example 2) and 25.0 g of methyl isocyanate was refluxed for 8.5 hours. After completion of the reaction, excess methyl isocyanate was evaporated from the reaction mixture and then the residue was purified by column chromatography through silica gel eluted with a 24:12:2:1 by volume mixture of ethyl acetate, benzene, triethylamine and ethanol and then by recrystallisation from ethanol. The desired Compound No. 31 was obtained in the form of white crystals, melting point 238°-242° C.

WORKUP

后处理

temperaturewas refluxed for 8.5 hours
customwas evaporated from the reaction mixture
customthe residue was purified by column chromatography through silica gel
washeluted with a 24:12:2:1 by volume mixture of ethyl acetate, benzene, triethylamine and ethanol
customby recrystallisation from ethanol
custom31 was obtained in the form of white crystals, melting point 238°-242° C.

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-40fe96a0f1fd4737b240263bef95ee68
来源数据集: uspto-grants-1979_07
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04162246
来源说明: uspto-grants-1979_07

反应 SMILES

[OH:1][CH:2]([CH2:41][N:42]1[C:46](=[O:47])[C:45]2([CH2:52][C:51]([CH3:54])([CH3:53])[NH:50][C:49]([CH3:56])([CH3:55])[CH2:48]2)[NH:44][C:43]1=[O:57])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH:22]([OH:40])[CH2:23][N:24]3[C:28](=[O:29])[C:27]4([CH2:34][C:33]([CH3:36])([CH3:35])[NH:32][C:31]([CH3:38])([CH3:37])[CH2:30]4)[NH:26][C:25]3=[O:39])=[CH:16][CH:15]=2)([CH3:13])[CH3:12])=[CH:7][CH:6]=1.[CH3:58][N:59]=[C:60]=[O:61]>>[CH3:58][NH:59][C:60]([O:40][CH:22]([CH2:23][N:24]1[C:28](=[O:29])[C:27]2([CH2:34][C:33]([CH3:35])([CH3:36])[NH:32][C:31]([CH3:37])([CH3:38])[CH2:30]2)[NH:26][C:25]1=[O:39])[CH2:21][O:20][C:17]1[CH:18]=[CH:19][C:14]([C:11]([C:8]2[CH:7]=[CH:6][C:5]([O:4][CH2:3][CH:2]([O:1][C:25](=[O:39])[NH:24][CH3:23])[CH2:41][N:42]3[C:46](=[O:47])[C:45]4([CH2:48][C:49]([CH3:56])([CH3:55])[NH:50][C:51]([CH3:54])([CH3:53])[CH2:52]4)[NH:44][C:43]3=[O:57])=[CH:10][CH:9]=2)([CH3:13])[CH3:12])=[CH:15][CH:16]=1)=[O:61]