碘甲烷 → 乙酰胆碱碘化物

HRID 1275370

反应方程式

HRID 1275370 反应方程式
[CH3:1][N:2]([CH2:4][CH2:5][OH:6])[CH3:3].[3H][CH2:8][C:9](ON1C(=O)C2=CC=CC=C2C1=O)=[O:10].[CH3:23][I:24]>C(#N)C>[I-:24].[C:9]([O:6][CH2:5][CH2:4][N+:2]([CH3:23])([CH3:3])[CH3:1])(=[O:10])[CH3:8]

参与物

5

反应物 3

HCID 6328碘甲烷HCID 7902N,N-二甲基乙醇胺HCID 10488521HCID 10488521，化合物

产物 1

HCID 75271乙酰胆碱碘化物

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂2 次

反应条件

温度
75 °C

实验过程

N,N-Dimethylaminoethanol (4 μL, 0.04 mmole) was dissolved in dry acetonitrile (0.25 mL) and was placed in a reaction vessel connected to the vacuum line. N-tritioacetoxyphthalimide (0.04 mmole, specific activity 13 Ci/mmole) in dry acetonitrile (0.8 mL) was then added through the side-arm of the reaction vessel. The mixture was heated at 75° C. for 2 hours under N2, then brought to room temperature and methyl iodide (20 μL) was injected. The mixture was stirred for 1 hour. The solvent and excess of methyl iodide was evaporated under vacuum. Deuteriated water (0.5 mL) was added and removed. D2O (1 mL) was then added to the residue and filtered and the product was analyzed by 1H and 3H NMR spectroscopy.

后处理

  1. customwas placed in a reaction vessel
  2. custombrought to room temperature
  3. customThe solvent and excess of methyl iodide was evaporated under vacuum
  4. additionDeuteriated water (0.5 mL) was added
  5. customremoved
  6. additionD2O (1 mL) was then added to the residue
  7. filtrationfiltered

来源与证据

ORD记录
ord-9a70f0f9c217492ba5b74e4a4ac0990c
来源数据集
uspto-grants-2000_12
专利号
US06160128

关联笔记

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