海萝胶 → HCID 178457009，化合物

HRID 38706

反应方程式

HRID 38706 反应方程式
[CH:1]([NH2:4])([CH3:3])[CH3:2].[C:5]1([N:11]=[C:12]=[S:13])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.N1C=CC=CC=1.Br[CH2:21][C:22](OC)=[O:23].Cl>CO>[C:5]1([N:11]2[C:22](=[O:23])[CH2:21][S:13]/[C:12]/2=[N:4]\[CH:1]([CH3:3])[CH3:2])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参与物

7

反应物 5

HCID 313海萝胶HCID 1049吡啶HCID 6363异丙胺HCID 7673硫代异氰酸苯酯HCID 60984溴乙酸甲酯

产物 1

HCID 178457009HCID 178457009，化合物

试剂、催化剂与溶剂 1

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

实验过程

To a solution of isopropylamine (1.31 g, 22.19 mmol) in methanol (25 mL) is added portionwise phenylisothiocyanate (3.0 g, 22.19 mmol). The solution which becomes slightly warm during the addition is stirred at rt for 4 h before pyridine (2.63 g, 33.29 mmol) and methyl bromoacetate (3.39 g, 22.19 mmol) is added. The mixture is stirred for another 16 h at rt before it is poured onto 1 N aq. HCl (100 mL) and extracted with diethyl ether (150 mL). The aq. layer is neutralised by adding sat. aq. NaHCO3 and extracted with diethyl ether (4×150 mL). The organic extracts are dried over MgSO4 and evaporated. The remaining solid is suspended in diethyl ether/heptane, filtered off, washed with additional diethyl ether/heptane and dried to give 3-phenyl-2-[(Z)-isopropylimino]-thiazolidin-4-one.

后处理

  1. temperatureThe solution which becomes slightly warm during the addition
  2. additionis added
  3. extractionextracted with diethyl ether (150 mL)
  4. additionby adding sat. aq. NaHCO3
  5. extractionextracted with diethyl ether (4×150 mL)
  6. dry with materialThe organic extracts are dried over MgSO4
  7. customevaporated
  8. filtrationfiltered off
  9. washwashed with additional diethyl ether/heptane
  10. customdried

来源与证据

ORD记录
ord-4eb34ee1f82545c0b033ad06916456d0
来源数据集
uspto-grants-2013_09
专利号
US08524752B2

关联笔记

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