反応式
C(=O)([O-])[O-].[Na+].[Na+].C(O)(=O)[CH2:8][CH3:9].[C:12](OC=C)(=O)[CH3:13].[O:18]1[CH2:21][C:20]([CH2:24][OH:25])([CH2:22][OH:23])[CH2:19]1>C1(C)C=CC=CC=1>[CH:12]([O:23][CH2:22][C:20]1([CH2:24][O:25][CH:8]=[CH2:9])[CH2:21][O:18][CH2:19]1)=[CH2:13]参加物
実験手順
A mixture (280 mL) of 24.9 g (0.23 mol) of sodium carbonate and toluene was heated to a temperature of 95° C., and 1.4 g of propionic acid was added dropwise to the mixture. Next, maintaining the temperature of the reaction mixture, 16 g of vinyl acetate was added dropwise to the mixture, and fifteen minutes later, further the mixture was combined with 1.27 g (1.9 mmol) of di-μ-chlorobis(1,5-cyclooctadiene)diiridium(I) [Ir(cod)Cl]2. Next, 40 g (0.19 mol) of oxetane-3,3-dimethanol was added dropwise for three hours, and a reaction was carried out in a nitrogen atmosphere while adding dropwise 79.8 g of vinyl acetate and maintaining the temperature of the reaction mixture. After the completion of dropwise addition, the mixture was stirred for one hour. As the result of gas chromatography analysis of the mixture, it is confirmed that there were produced 3,3-bis(vinyloxymethyl)oxetane represented by following Formula (10) in a yield of 90% and (3-vinyloxymethyloxetan-3-yl)methanol in a yield of 2%. Purification of the reaction mixture by distillation yielded 31 g of 3,3-bis(vinyloxymethyl)oxetane with a purity of 99%.
後処理
- additionwas added dropwise to the mixture
- additionwas added dropwise to the mixture, and fifteen minutes later
- temperaturemaintaining the temperature of the reaction mixture
- additionAfter the completion of dropwise addition
- customAs the result of gas chromatography analysis of the mixture, it
出典と根拠
- ORDレコード
- ord-d8775964c06442a8b9e99bb597776ef8
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07985866B2
関連ノート
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