乙醚 → 4-甲脒基氯化吡啶

HRID 10237

反应方程式

HRID 10237 反应方程式
[Na].[C:2]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)#[N:3].[Cl-:10].[NH4+:11].C(OCC)C>CO>[ClH:10].[C:2]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)(=[NH:11])[NH2:3]

参与物

6

反应物 4

HCID 3283乙醚HCID 75064-氰基吡啶HCID 25517氯化铵HCID 5360545钠

产物 1

HCID 27768444-甲脒基氯化吡啶收率 93%

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 sodium (0.23 g) in methanol (40 ml) was added 4-cyanopyridine (10.62 g) at r.t. Stirring was continued for 6 h followed by the addition of ammoniumchloride (5.9 g) and stirring was continued for another 10 h. Then, diethylether (120 ml) was added and the precipitate was filtered off after 30 min and washed with diethylether (20 ml). The product was dried under high vacuum. 4-Amidino-pyridine hydrochloride (14.95 g) was obtained as a white powder.

后处理

  1. stirringstirring
  2. waitwas continued for another 10 h
  3. filtrationthe precipitate was filtered off after 30 min
  4. washwashed with diethylether (20 ml)
  5. customThe product was dried under high vacuum

来源与证据

ORD记录
ord-eabe532b36c040a6b450ec034d5b8835
来源数据集
uspto-grants-2006_08
专利号
US07094781B2

关联笔记

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