过碘酸钾 → N-叔丁氧羰基-2-氨基乙醛

HRID 51183笔记

反应方程式

HRID 51183 反应方程式
[C:1]([NH:8][CH2:9][CH:10]([OH:13])CO)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].I([O-])(=O)(=O)=O.[K+]>O>[C:1]([NH:8][CH2:9][CH:10]=[O:13])([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]

参与物

4

反应物 2

HCID 516896过碘酸钾HCID 4206999N-(2,3-二羟基丙基)氨基甲酸叔丁酯

产物 1

HCID 4247255N-叔丁氧羰基-2-氨基乙醛

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

3-Bocamino-1,2-propanediol (144.7 g; 0.757 mol) was suspended in water (750 ml) and potassium periodate (191.5 g; 0.833 mol) was added. The mixture was stirred under nitrogen for 2.5 h and the precipitated potassium iodate was removed by filtration and washed once with water (100 ml). The aqueous phase was extracted with chloroform (6×400 ml). The chloroform extracts were dried and evaporated to dryness, in vacuo. Yield 102 g (93%) of an oil. The (bocamino)acetaldehyde was purified by kugelrohr distillation at 84° C. and 0.3 mmHg in two portions. The yield 79 g (77%) of a colorless oil.

后处理

  1. customthe precipitated potassium iodate was removed by filtration
  2. washwashed once with water (100 ml)
  3. extractionThe aqueous phase was extracted with chloroform (6×400 ml)
  4. dry with materialThe chloroform extracts were dried
  5. customevaporated to dryness, in vacuo
  6. distillationThe (bocamino)acetaldehyde was purified by kugelrohr distillation at 84° C.

来源与证据

ORD记录
ord-be7e821a61eb41e3be15a2c1f4638904
来源数据集
uspto-grants-2004_03
专利号
US06713602B1

反应笔记

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