ubiquitin cross-reactive protein → N-[2-(Diethylamino)ethyl]-N-methyl-N'-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea citrate hydrate

HRID 4228

反应方程式

HRID 4228 反应方程式
[CH3:1][CH:2]([N:4]([CH2:8][CH2:9][S:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:12])=[O:11])[C:5](Cl)=[O:6])[CH3:3].[CH2:19]([N:21]([CH2:26][CH3:27])[CH2:22][CH2:23][NH:24][CH3:25])[CH3:20].C(N(CC)CC)C.[C:35]([OH:47])(=[O:46])[CH2:36][C:37]([CH2:42][C:43]([OH:45])=[O:44])([C:39]([OH:41])=[O:40])[OH:38]>O1CCCC1.CO.CCOCC>[OH2:6].[C:35]([OH:47])(=[O:46])[CH2:36][C:37]([CH2:42][C:43]([OH:45])=[O:44])([C:39]([OH:41])=[O:40])[OH:38].[CH2:19]([N:21]([CH2:26][CH3:27])[CH2:22][CH2:23][N:24]([CH3:25])[C:5]([N:4]([CH:2]([CH3:3])[CH3:1])[CH2:8][CH2:9][S:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:12])=[O:11])=[O:6])[CH3:20]

参与物

8

反应物 4

HCID 311ubiquitin cross-reactive proteinHCID 8471三乙胺HCID 66034N,N-二乙基-N'-甲基乙二胺HCID 13655164N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride

产物 1

HCID 70419038N-[2-(Diethylamino)ethyl]-N-methyl-N'-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea citrate hydrate

试剂、催化剂与溶剂 3

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂HCID 3283乙醚溶剂HCID 8028四氢呋喃溶剂

实验过程

A mixture of 6.65 g (0.023 mole) of N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride; 3.0 g (0.023 mole) of N,N-diethyl-N'-methylethylenediamine and triethylamine (2.7 g, 0.0267 mole) in 400 ml of tetrahydrofuran was stirred at room temperature for 10 hr. The solvent was removed in vacuo, and the residue was dissolved in a 60/40 mixture of ether and methylene chloride. This solution was extracted with several portions of water and was dried over magnesium sulfate. The solvent was removed in vacuo to give an oil. This was dissolved in methanol, an excess of citric acid was added, and ether was added. A solid precipitated to give 11.08 g (82.4%) of white, crystalline solid; m.p. 77°-82° C.

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in a 60/40 mixture of ether and methylene chloride
  3. extractionThis solution was extracted with several portions of water
  4. dry with materialwas dried over magnesium sulfate
  5. customThe solvent was removed in vacuo
  6. customto give an oil
  7. customA solid precipitated
  8. customto give 11.08 g (82.4%) of white, crystalline solid

来源与证据

ORD记录
ord-1bbdfdf4f42246edb2dbfdf161a6a0b2
来源数据集
uspto-grants-1988_02
专利号
US04724235

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