Lactic Acid → HCID 10130434, compound

HRID 1418669Notes

Reaction equation

HRID 1418669 reaction equation
[C:1]([OH:6])(=[O:5])[CH:2]([CH3:4])[OH:3].[C:7]1(=[O:14])[O:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1.[Si]([O-])([O-])([O-])[O-].[Al+3].[Si]([O-])([O-])([O-])[O-].[Si]([O-])([O-])([O-])[O-].[Al+3].[Al+3].[Al+3]>>[C:1]([OH:6])(=[O:5])[CH:2]([CH3:4])[OH:3].[C:7]1(=[O:14])[O:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1

Participants

4

Reactant 3

HCID 612Lactic AcidHCID 10401epsilon-CAPROLACTONEHCID 21981400Tetraaluminum;trisilicate

Product 1

HCID 10130434HCID 10130434, compound

Conditions

Temperature
150 °C

Procedure

The lactide obtained in Example 2 (17 g) and ε-caprolactone (3 g) were put into a 100-ml reaction vessel equipped with a stirrer and a nitrogen-introducing tube. After substitution of nitrogen gas was carried out three times, the mixture was molten by stirring at 150° C. for 3 hours in a stream of nitrogen. To the resulting mixture was added 0.4 g of synthetic light aluminum silicate (Tomita Pharmaceutical Co., Ltd.), and the temperature was raised to 195°±5° C. The pressure was reduced gradually to 20 mmHg over 30 minutes, followed by stirring at 195°±5° C. for 3 hours. After the pressure was reduced gradually to 1 mmHg over 30 minutes, the mixture was stirred at 195°±5° C. for 7 hours to give lactic acid-caprolactone copolymer in the molten state. The product was cooled to room temperature to give 12.11 g of light brown copolymer. The weight-average molecular weight of this copolymer was 82,000.

Workup

  1. customequipped with a stirrer
  2. additiona nitrogen-introducing tube
  3. temperaturethe temperature was raised to 195°±5° C
  4. waitThe pressure was reduced gradually to 20 mmHg over 30 minutes
  5. stirringby stirring at 195°±5° C. for 3 hours
  6. waitAfter the pressure was reduced gradually to 1 mmHg over 30 minutes
  7. stirringthe mixture was stirred at 195°±5° C. for 7 hours

Sources & evidence

ORD record
ord-d262203b0b8f4c28aa3fee7874c6aeab
Source dataset
uspto-grants-1999_03
Patent number
US05883222

Reaction notes

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