Propylene Glycol → TMC caprolactone

HRID 2264

反応式

HRID 2264 の反応式
[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:9]1(=[O:15])[O:14][CH2:13][CH2:12][CH2:11][O:10]1.C(O)C(O)C.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.[C:9]1(=[O:15])[O:14][CH2:13][CH2:12][CH2:11][O:10]1

参加物

6

反応物 4

HCID 1030Propylene GlycolHCID 93182-ethylhexanoic acid tin(II) saltHCID 10401epsilon-CAPROLACTONEHCID 123834Trimethylene carbonate

生成物 1

HCID 11275958TMC 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, 51.0 grams (0.50 mole) of trimethylene carbonate, 4.4 mL (60mmol) of propylene glycol (USP), and 0.10 mL (34 μmol) of a 0.33M solution of stannous octoate in toluene. The flask was fitted with a flame dried mechanical stirrer. The flask 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 80° C. for about 16 hours to remove any unreacted monomer. The copolymer had an inherent viscosity of 0.20 dL/g in HFIP at 25° C. The copolymer was a viscous liquid at room temperature.

後処理

  1. customA flame dried
  2. customThe flask was fitted with a flame
  3. customdried mechanical stirrer
  4. customThe flask 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 80° 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-a39ac505275c4aed98cfeb34fa86c787
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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