HRID329830

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID280

Carbon dioxide

CO2

$结构：O=C(O)/C=C\C(=O)O$

HCID444266

Maleic acid

C4H4O4

结构：CCCC[P+](C)(CCCC)CCCC.CCCC[P+](C)(CCCC)CCCC.O=C([O-])[O-]

HCID86743661

未命名化合物

PRODUCTS

生成物

HCID13831

Tributylphosphine

C12H27P

$结构：CCCC[P+](C)(CCCC)CCCC.CCCC[P+](C)(CCCC)CCCC.O=C([O-])/C=C\C(=O)[O-]$

HCID86743660

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID962

Water

H2O

PROCEDURE

实验过程

In 10.0 g of water was dissolved 10.0 g of tri-n-butylmethylphosphonium carbonate obtained as in Example 12 (1st step) and a solution of 4.2 g of maleic acid dissolved in 5.0 g of water was gradually added to the solution, whereby carbon dioxide simultaneously generated vigorously. For more completely removing carbon dioxide, degassing was performed for 2 hours at 40° C. and 20 mmHg and after confirming carbonate ions being less than 2 ppm, water was distilled off. The residue formed was recrystallized from methyl ethyl ketone to produce 1-1.2 g (94.1% of the theoretical yield, yield of 59.8% to tri-n-butylphosphine) of tri-n-butylmethylphosphonium monomaleate.

WORKUP

后处理

customobtained as in Example 12 (1st step)
customFor more completely removing carbon dioxide, degassing
distillationwas distilled off
customThe residue formed
customwas recrystallized from methyl ethyl ketone

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-5ab61bab052f4c1da1c1530b5098c1ce
来源数据集: uspto-grants-1990_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04892944

反应 SMILES

C(=O)([O-])[O-].[CH2:5]([P+:9]([CH2:15][CH2:16][CH2:17][CH3:18])([CH2:11][CH2:12][CH2:13][CH3:14])[CH3:10])[CH2:6][CH2:7][CH3:8].[CH2:19]([P+:23]([CH3:32])([CH2:28][CH2:29][CH2:30][CH3:31])[CH2:24][CH2:25][CH2:26][CH3:27])[CH2:20][CH2:21][CH3:22].[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([OH:38])=[O:37].C(=O)=O>O>[CH2:15]([P:9]([CH2:5][CH2:6][CH2:7][CH3:8])[CH2:11][CH2:12][CH2:13][CH3:14])[CH2:16][CH2:17][CH3:18].[C:33]([O-:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([O-:38])=[O:37].[CH2:28]([P+:23]([CH2:19][CH2:20][CH2:21][CH3:22])([CH2:24][CH2:25][CH2:26][CH3:27])[CH3:32])[CH2:29][CH2:30][CH3:31].[CH2:5]([P+:9]([CH3:10])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:15][CH2:16][CH2:17][CH3:18])[CH2:6][CH2:7][CH3:8]