Glycerol → L-lactide epsilon-caprolactone

HRID 2257

反応式

HRID 2257 の反応式
[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:9][C@@H:10]1[O:17][C:15](=[O:16])[C@H:14]([CH3:18])[O:13][C:11]1=[O:12].OCC(CO)O.CCCCC(C([O-])=O)CC.CCCCC(C([O-])=O)CC.[Sn+2]>C1(C)C=CC=CC=1>[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:9][C@@H:10]1[O:17][C:15](=[O:16])[C@H:14]([CH3:18])[O:13][C:11]1=[O:12]

参加物

6

反応物 4

HCID 753GlycerolHCID 93182-ethylhexanoic acid tin(II) saltHCID 10401epsilon-CAPROLACTONEHCID 107983Lactide, L-

生成物 1

HCID 131710947L-lactide epsilon-caprolactone

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
160 °C

実験手順

A flame dried, 250 mL, round bottom single neck flask was charged with 57.1 grams (0.50 mole) of ε-caprolactone, 72.1 grams (0.50 mole) of L-lactide, 4.00 mL (55 mmol) of distilled glycerol, and 0.10 mL (34 μmol) of a 0.33M stannous octoate solution in toluene. The flask was fitted with a flame dried mechanical stirrer. The reactor was purged with nitrogen three times before venting with nitrogen. The reaction mixture was heated to 160° C. and maintained at this temperature for about 18-20 hours. The copolymer was dried under vacuum (0.1 mm Hg) at 110° C. for about 16 hours to remove any unreacted monomer. The copolymer had an inherent viscosity of 0.14 dL/g in hexafluoroisoproponal (HFIP) at 25° C. The copolymer was a liquid at room temperature. The molar ratio of PCL/PLA was found to be 53.7/46.3 by proton NMR.

後処理

  1. customA flame dried
  2. customThe flask was fitted with a flame
  3. customdried mechanical stirrer
  4. customThe reactor was purged with nitrogen three times
  5. temperaturemaintained at this temperature for about 18-20 hours
  6. customThe copolymer was dried under vacuum (0.1 mm Hg) at 110° C. for about 16 hours
  7. customto remove any unreacted monomer
  8. customat 25° C
  9. customat room temperature

出典と根拠

ORDレコード
ord-f9e0a5c87bd84b7d80805188d5773375
出典データセット
uspto-grants-1998_03
特許番号
US05728752

関連ノート

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