HRID324397

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1

HCID87949

p-Anisyldithiophosphonic anhydride

C14H14O2P2S4

结构：CCOC(=O)c1coc(Cn2cc(C3c4ccc(C)cc4C=Cc4oc(CC)nc43)c(=O)[nH]c2=O)n1

HCID131722501

未命名化合物

PRODUCTS

生成物

结构：CCOC(=O)c1coc(Cn2cc(C3c4ccc(C)cc4C=Cc4oc(CC)nc43)c(=S)[nH]c2=O)n1

HCID131722502

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID31275

1,4-Dioxane

C4H8O2

PROCEDURE

实验过程

A mixture of the product of step (i) (1.26 g) and Lawesson's reagent (1.56 g) in 1,4-dioxane (30 ml) was heated at reflux for 16 hours. The solvent was evaporated under reduced pressure. The residue was partitioned between ethyl acetate and saturated brine. The organic phase was collected, dried (MgSO4) and solvent evaporated under reduced pressure. Purification was by chromatography eluting with 50% ethyl acetate in toluene.

WORKUP

后处理

temperaturewas heated
temperatureat reflux for 16 hours
customThe solvent was evaporated under reduced pressure
customThe residue was partitioned between ethyl acetate and saturated brine
customThe organic phase was collected
dry with materialdried (MgSO4) and solvent
customevaporated under reduced pressure
customPurification
washeluting with 50% ethyl acetate in toluene

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-4db8ff9f2ae548ec8da67ebb69ab2234
来源数据集: uspto-grants-2001_04
DOI: 10.6084/m9.figshare.5104873.v1
专利: US06218376B1
来源说明: uspto-grants-2001_04

反应 SMILES

[CH2:1]([C:3]1[O:4][C:5]2[CH:12]=[CH:11][C:10]3[CH:13]=[C:14]([CH3:17])[CH:15]=[CH:16][C:9]=3[CH:8]([C:18]3[C:19](=O)[NH:20][C:21](=[O:35])[N:22]([CH2:24][C:25]4[O:26][CH:27]=[C:28]([C:30]([O:32][CH2:33][CH3:34])=[O:31])[N:29]=4)[CH:23]=3)[C:6]=2[N:7]=1)[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:46])=CC=1>O1CCOCC1>[CH2:1]([C:3]1[O:4][C:5]2[CH:12]=[CH:11][C:10]3[CH:13]=[C:14]([CH3:17])[CH:15]=[CH:16][C:9]=3[CH:8]([C:18]3[C:19](=[S:46])[NH:20][C:21](=[O:35])[N:22]([CH2:24][C:25]4[O:26][CH:27]=[C:28]([C:30]([O:32][CH2:33][CH3:34])=[O:31])[N:29]=4)[CH:23]=3)[C:6]=2[N:7]=1)[CH3:2]