海萝胶 → γ-丁内酯

HRID 34887

反应方程式

HRID 34887 反应方程式
[C:1]1(=[O:6])[O:5][CH2:4][CH2:3][CH2:2]1.[C:7]([Cl:10])(Cl)=[O:8].[ClH:11]>[Cl-].C[N+](C)(C)CC1C=CC=CC=1>[Cl:11][CH2:3][CH2:2][CH2:1][C:7]([Cl:10])=[O:8].[C:1]1(=[O:6])[O:5][CH2:4][CH2:3][CH2:2]1

参与物

6

反应物 3

HCID 313海萝胶2 次HCID 6371光气3 次HCID 7302γ-丁内酯

产物 2

HCID 7302γ-丁内酯HCID 783704-氯丁酰氯

试剂、催化剂与溶剂 1

HCID 5963苄基三甲基氯化铵催化剂

反应条件

温度
130 °C

实验过程

430 parts of 4-butyrolactone and 47 parts of trimethylbenzylammonium chloride are initially taken in a 1 l stirred reactor which is equipped with a thermometer, inlet tubes for phosgene and hydrogen chloride and 2 low-temperature coolers set at -20° C. and -70° C. respectively. The mixture is heated to 130° C. 560 parts of phosgene and 120 parts of hydrogen chloride are passed in over 5.5 hours. Thereafter, nitrogen is passed in until the reaction mixture no longer contains any phosgene. Working up by distillation gives 620 g of 4-chlorobutyryl chloride and 30.5 g of butyrolactone. The distillation residue of 75 g, which consists of the catalyst and chlorobutyroyloxybutyryl chloride, can be reused for further batches. The yield of 4-chlorobutyryl chloride is 88 mol %, based on butyrolactone used.

后处理

  1. customset at -20° C. and -70° C.
  2. customare passed in over 5.5 hours
  3. distillationWorking up by distillation

来源与证据

ORD记录
ord-6b818966f76a4387b4c35f6e99b7421f
来源数据集
uspto-grants-1988_08
专利号
US04764309

关联笔记

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