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HRID963853

反应详情

EQUATION

反应方程式

HRID 963853 的结构方程式

REACTANTS

反应物

3
结构：CCN(CC)CC
HCID8471

Triethylamine

C6H15N

结构：CC(C)(C)OC(=O)NCC1CCNCC1
HCID723429

tert-Butyl [(piperidin-4-yl)methyl]carbamate

C11H22N2O2

结构：N=C(N)S(=O)(=O)O
HCID9877361

Methanesulfonic acid, aminoimino-

CH4N2O3S

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)NCC1CCN(C=NN)CC1.CC(C)(C)OC(=O)NCC1CCN(C=NN)CC1.O=S(O)O
HCID131720709

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

PROCEDURE

实验过程

A solution of 130 g of 1,1-dimethylethyl (4piperidinylmethyl)-carbamate in 1300 ml of DMF is treated with 138 ml of triethylamine and 61.8 g of formamidinesulfonic acid and the mixture is stirred at room temperature overnight. The precipitated material is filtered, suspended in 500 ml of ethanol, again filtered off and dried. There are obtained 65.6 g of tert-butyl 1-(aminoimino-methyl)-piperidin-4-ylmethylcarbamate hemisulfite, MS (ISP): 257.4 (M+H)+.

WORKUP

后处理

  1. filtrationThe precipitated material is filtered
  2. filtrationagain filtered off
  3. customdried