盐酸 → (氯甲酰基)乙酸乙酯

HRID 52688笔记

反应方程式

HRID 52688 反应方程式
C[C:2](C)([O-:4])C.[K+].[Cl:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].C(OCC)=O.Cl>C1COCC1.C(OCC)C>[Cl:7][CH:8]([CH:2]=[O:4])[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参与物

7

反应物 4

HCID 313盐酸HCID 7751氯乙酸乙酯HCID 8025甲酸乙酯HCID 23665647叔丁醇钾

产物 1

HCID 118030(氯甲酰基)乙酸乙酯

试剂、催化剂与溶剂 2

HCID 3283乙醚溶剂HCID 8028四氢呋喃溶剂3 次

反应条件

温度
0 °C

实验过程

To a three neck 2 L round bottom flask charged with potassium t-butoxide (0.5 mol, 500 mL of a 1M solution in THF) and 500 mL of dry THF cooled to 0° C. was added dropwise from an addition funnel a solution of ethyl chloroacetate (0.5 mol, 53.5 mL) and ethyl formate (0.5 mol, 40.4 mL), in 200 mL of THF over 3 hours. After completion of addition, the reaction mixture was stirred for 1 hour and allowed to stand overnight. The resulting solid was diluted with diethyl ether and cooled in an ice bath. Then, the pH was lowered to approximately 3 using 6N HCl. The organic phase was separated, and the aqueous layer was washed 3 times with diethyl ether. The combined ethereal portions were dried over NaSO4, and concentrated in vacuo. The crude desired compound was stored at -30° C. and used without further purification.

后处理

  1. additionAfter completion of addition
  2. waitto stand overnight
  3. temperaturecooled in an ice bath
  4. customThe organic phase was separated
  5. washthe aqueous layer was washed 3 times with diethyl ether
  6. dry with materialThe combined ethereal portions were dried over NaSO4
  7. concentrationconcentrated in vacuo
  8. customwas stored at -30° C.
  9. customused without further purification

来源与证据

ORD记录
ord-3b5787ed4fa44e35960500a1d5aaac7c
来源数据集
uspto-grants-1997_04
专利号
US05616720

反应笔记

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