Gamma-Butyrolactone → HCID 15767531, compound
Reaction equation
[CH2:1]([O:5][CH2:6][CH2:7][CH2:8][NH2:9])[CH2:2][CH2:3][CH3:4].[C:10]1(=O)[O:14][CH2:13][CH2:12][CH2:11]1>>[CH2:1]([O:5][CH2:6][CH2:7][CH2:8][N:9]1[CH2:10][CH2:11][CH2:12][C:13]1=[O:14])[CH2:2][CH2:3][CH3:4]Participants
3
Conditions
- Temperature
- 275 °C
Procedure
360 grams of butoxypropylamine (2.75 moles) and 250 grams of butyrolactone (3.0 moles) were charged to a 1-liter stainless steel autoclave. After purging, the mixture was heated to 275° C. for six hours. The reactor was then cooled and the product discharged. The product was distilled with a simple Vigreux column, initially at atmospheric pressure to remove by-product water and then under vacuum (<1 mm) to recover the product. Butoxypropyl Pyrrolidone distills at about 135° C. to 145° C. under these conditions. The recovery was 391.2 grams of>98% pure Butoxypropyl Pyrrolidone.
Workup
- customAfter purging
- temperatureThe reactor was then cooled
- distillationThe product was distilled with a simple Vigreux column, initially at atmospheric pressure
- customto remove by-product water
- customunder vacuum (<1 mm) to recover the product
- distillationButoxypropyl Pyrrolidone distills at about 135° C. to 145° C. under these conditions
Sources & evidence
- ORD record
- ord-75d11de14ffa412db492ba6279f9d9b4
- Source dataset
- uspto-grants-1995_01
- Patent number
- US05385948
Reaction notes
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