反应 #543573

ord-051f0f6500414de0a26c22475a10310e

反应方程式

CI
Methyl iodide
CC(C)(C)OC(=O)N1CCOC(C(=O)O)C1
4-(tert-butoxycarbonyl)-2-morpholinecarboxylic acid
O=C([O-])[O-].[K+].[K+]
potassium carbonate
COC(=O)C1CN(C(=O)OC(C)(C)C)CCO1
crude product
收率 143.3%
COC(=O)C1CN(C(=O)OC(C)(C)C)CCO1
4-(tert-Butyl) 2-methyl 2,4-morpholinedicarboxylate
收率 143.3%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤filtered through Celite
  2. 2
    浓缩concentrated
  3. 3
    其他The residue was partitioned between dichloromethane and water
  4. 4
    干燥The organic phase was dried over magnesium sulfate
  5. 5
    浓缩concentrated

实验过程

Methyl iodide (9.38 ml, 150 mmol) was added to a suspension of 4-(tert-butoxycarbonyl)-2-morpholinecarboxylic acid (14.5 g, 62.6 mmol) and dry potassium carbonate (17.3 g, 125 mmol) in dry dimethylformamide (DMF) (360 ml). The mixture was stirred over night, filtered through Celite and concentrated. The residue was partitioned between dichloromethane and water. The organic phase was dried over magnesium sulfate and concentrated to give 22 g of crude product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07186718B2uspto-grants-2007_03