p-Toluenesulfonic acid → HCID 20194899、化合物

HRID 653511ノート

反応式

HRID 653511 の反応式
[CH3:1][O:2][C:3]([C:5]([C:15]([O:17][CH3:18])=[O:16])([CH2:8][CH2:9][CH:10]([O:13][CH3:14])[O:11]C)[CH2:6]O)=[O:4].C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)([O-])[O-].[K+].[K+]>C1C=CC=CC=1>[CH3:14][O:13][CH:10]1[O:11][CH2:6][C:5]([C:3]([O:2][CH3:1])=[O:4])([C:15]([O:17][CH3:18])=[O:16])[CH2:8][CH2:9]1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 11430Potassium CarbonateHCID 20194908HCID 20194908、化合物

生成物 1

HCID 20194899HCID 20194899、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of dimethyl-1-hydroxy-5,5-dimethoxypentane-2,2-dicarboxylate made in accordance with Example I (8.4 g, 0.032 mol), p-toluenesulfonic acid (0.052 g, 0.027 mmol) in dry benzene (600 ml) was allowed to reflux through a Soxhlet extractor for 2 hours. The Soxhlet thimble was charged with Type 4 A molecular sieves (ca 20 g). After the mixture was cooled to room temperature, anhydrous potassium carbonate (7 g, 0.05 mol) was added, and the mixture was stirred for 30 min. The mixture was filtered and the solvent was removed by a rotary evaporator. The residual amber oil was distilled under reduced pressure. Yield of the product, which had a bp of 95°-100° C. (1 mmHg), was 84%.

後処理

  1. temperatureto reflux through a Soxhlet extractor for 2 hours
  2. additionThe Soxhlet thimble was charged with Type 4 A molecular sieves (ca 20 g)
  3. filtrationThe mixture was filtered
  4. customthe solvent was removed by a rotary evaporator
  5. distillationThe residual amber oil was distilled under reduced pressure

出典と根拠

ORDレコード
ord-459bfeaff7dc4019ad42865d378cc1c8
出典データセット
uspto-grants-1987_06
特許番号
US04677190

反応ノート

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