HRID1660540

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID8471

Triethylamine

C6H15N

HCID8857

Ethyl acetate

C4H8O2

结构：CCC(Oc1ccc(C(C)(C)CC)cc1C(C)(C)CC)C(=O)Nc1cccc(C(=O)NC2=NN(c3c(Cl)cc(Cl)cc3Cl)C(=O)C2n2cccn2)c1

HCID13668273

未命名化合物

HCID18444075

未命名化合物

PRODUCTS

生成物

结构：CCCC(=O)Oc1c(-n2cccn2)c(NC(=O)c2cccc(NC(=O)C(CC)Oc3ccc(C(C)(C)CC)cc3C(C)(C)CC)c2)nn1-c1c(Cl)cc(Cl)cc1Cl

HCID20556951

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8028

Tetrahydrofuran

C4H8O

2 次

PROCEDURE

实验过程

30.6 g of 3-{3-[2-(2,4-di-tert-amylphenoxy)butyramido]benzamido}-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-5-oxo-2-pyrazoline (prepared by the method described in German Patent Application (OLS) No. 2,536,191) was dissolved in 100 ml of tetrahydrofuran and 5 g of triethylamine was added. To the solution, a solution containing 3.5 g of butanoyloxy chloride dissolved in 10 ml of tetrahydrofuran was dropwise added. After the addition of the solution, the mixture was stirred for 1 hour. 500 ml of ethyl acetate was added to the reaction mixture and washed several times with water. The oil layer was dried with anhydrous sodium sulfate and concentrated. Upon crystallization of the residue from acetonitrile, 24 g of Coupler (5) was obtained. The melting point of the coupler was 63° to 68° C.

WORKUP

后处理

additionwas dropwise added
additionAfter the addition of the solution
washwashed several times with water
dry with materialThe oil layer was dried with anhydrous sodium sulfate
concentrationconcentrated
customUpon crystallization of the residue from acetonitrile, 24 g of Coupler (5)
customwas obtained
customwas 63° to 68° C.

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-b3fad9f1cffc42d2ba9d9de60a7fb7f4
来源数据集: uspto-grants-1981_12
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04308343
来源说明: uspto-grants-1981_12

反应 SMILES

[C:1]([C:6]1[CH:47]=[C:46]([C:48]([CH2:51][CH3:52])([CH3:50])[CH3:49])[CH:45]=[CH:44][C:7]=1[O:8][CH:9]([CH2:42][CH3:43])[C:10]([NH:12][C:13]1[CH:14]=[C:15]([CH:39]=[CH:40][CH:41]=1)[C:16]([NH:18][C:19]1[CH:23]([N:24]2[CH:28]=[CH:27][CH:26]=[N:25]2)[C:22](=[O:29])[N:21]([C:30]2[C:35]([Cl:36])=[CH:34][C:33]([Cl:37])=[CH:32][C:31]=2[Cl:38])[N:20]=1)=[O:17])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:60](OCl)(=[O:64])[CH2:61][CH2:62][CH3:63].C(OCC)(=O)C>O1CCCC1>[C:1]([C:6]1[CH:47]=[C:46]([C:48]([CH2:51][CH3:52])([CH3:49])[CH3:50])[CH:45]=[CH:44][C:7]=1[O:8][CH:9]([CH2:42][CH3:43])[C:10]([NH:12][C:13]1[CH:14]=[C:15]([CH:39]=[CH:40][CH:41]=1)[C:16]([NH:18][C:19]1[C:23]([N:24]2[CH:28]=[CH:27][CH:26]=[N:25]2)=[C:22]([O:29][C:60](=[O:64])[CH2:61][CH2:62][CH3:63])[N:21]([C:30]2[C:31]([Cl:38])=[CH:32][C:33]([Cl:37])=[CH:34][C:35]=2[Cl:36])[N:20]=1)=[O:17])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2]