Hydrochloric Acid → Gamma-Butyrolactone

HRID 34887

反応式

HRID 34887 の反応式
[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

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 6371Phosgene3 回HCID 7302Gamma-Butyrolactone

生成物 2

HCID 7302Gamma-ButyrolactoneHCID 783704-Chlorobutyryl chloride

試薬・触媒・溶媒 1

HCID 5963Benzyltrimethylammonium chloride触媒

反応条件

温度
130 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-6b818966f76a4387b4c35f6e99b7421f
出典データセット
uspto-grants-1988_08
特許番号
US04764309

関連ノート

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