Hydrochloric Acid → Gamma-Butyrolactone

HRID 34887

반응식

HRID 34887 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 6371Phosgene3회HCID 7302Gamma-Butyrolactone

생성물 2

HCID 7302Gamma-ButyrolactoneHCID 783704-Chlorobutyryl chloride

시약·촉매·용매 1

HCID 5963Benzyltrimethylammonium chloride촉매

반응 조건

온도
130 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-6b818966f76a4387b4c35f6e99b7421f
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764309

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