HRID1918244

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID525

Malic acid

C4H6O5

HCID1140

Toluene

C7H8

$结构：CCN(CC)CCNC(=O)c1c(C)[nH]c(/C=C2\C(=O)Nc3ccc(F)cc32)c1C$

HCID5329102

Sunitinib

C22H27FN4O2

PRODUCTS

生成物

$结构：CCN(CC)CCNC(=O)c1c(C)[nH]c(/C=C2\C(=O)Nc3ccc(F)cc32)c1C.O=C(O)C[C@H](O)C(=O)O$

HCID6456015

Sunitinib malate

C26H33FN4O7

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID13387

N-Methyl-2-pyrrolidone

C5H9NO

CONDITIONS

反应条件

温度: 0 °C

PROCEDURE

实验过程

1 g of sunitinib base was dissolved in 3 ml of N-methyl pyrrolidone, at RT 0.336 g of Malic acid added (as a solid): the solution was heated to 40° C. than 15 ml of toluene was added and precipitation was observed. The suspension was kept at 40° C. for 1 hour than cooled to 0° C., filtered and washed with toluene. Dried at 60° C. under vacuum for 16 h.

WORKUP

后处理

additionadded (as a solid): the solution
additionwas added
customprecipitation
filtrationfiltered
washwashed with toluene
customDried at 60° C. under vacuum for 16 h.

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-37ec831ba5254c55a2c895c3466e369c
来源数据集: uspto-grants-2013_12
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08618309B2
来源说明: uspto-grants-2013_12

反应 SMILES

[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:15]([CH3:16])=[C:14](/[CH:17]=[C:18]2/[C:19]3[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=3[NH:26][C:27]/2=[O:28])[NH:13][C:12]=1[CH3:29])=[O:10])[CH2:4][CH3:5].[C:30]([OH:38])(=[O:37])[CH:31]([CH2:33][C:34]([OH:36])=[O:35])[OH:32].C1(C)C=CC=CC=1>CN1CCCC1=O>[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:15]([CH3:16])=[C:14](/[CH:17]=[C:18]2/[C:19]3[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=3[NH:26][C:27]/2=[O:28])[NH:13][C:12]=1[CH3:29])=[O:10])[CH2:4][CH3:5].[CH2:33]([C:34]([OH:36])=[O:35])[C@H:31]([OH:32])[C:30]([OH:38])=[O:37]