Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 10877568、化合物
反応式
[CH3:1][Si:2]([CH3:17])([CH3:16])[C:3]#[C:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9]C1CCCCO1.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>CO>[CH3:17][Si:2]([CH3:1])([CH3:16])[C:3]#[C:4][CH2:5][CH2:6][CH2:7][CH2:8][OH:9]参加物
4
実験手順
1-Trimethylsilyl[6-(oxacyclohex-2-yloxy)]hex-1-yne (76 g, 300 mmol) and pyridinium p-toluenesulfonate (0.05 g) were heated at reflux in methanol (200 mL). After cooling the solvent was removed under reduced pressure, the residue was dissolved in methylene chloride and washed with water, brine and dried (MgSO4). Evaporation of the solvent under reduced pressure afforded a residue which was distilled (b.p. 96° C., 3 mm Hg) to give 37.6 g (64%) of the product.
後処理
- temperatureAfter cooling the solvent
- customwas removed under reduced pressure
- dissolutionthe residue was dissolved in methylene chloride
- washwashed with water, brine
- dry with materialdried (MgSO4)
- customEvaporation of the solvent under reduced pressure
- customafforded a residue which
- distillationwas distilled (b.p. 96° C., 3 mm Hg)
出典と根拠
- ORDレコード
- ord-bd69a0667ac1498f804d7bed6fd4d07d
- 出典データセット
- uspto-grants-1989_10
- 特許番号
- US04877779
反応ノート
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