Gamma-Butyrolactone → HCID 70588848、化合物

HRID 2049900ノート

反応式

HRID 2049900 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[C:6]3[CH:12]=[C:11]([OH:13])[CH:10]=[CH:9][C:7]=3[O:8][C:4]=2[CH:3]=1.[C:16]1(=[O:21])[O:20][CH2:19][CH2:18][CH2:17]1.[H-].[Na+].[H][H]>>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[C:6]3[CH:12]=[C:11]([O:13][CH:17]([CH2:18][CH3:19])[C:16]([OH:21])=[O:20])[CH:10]=[CH:9][C:7]=3[O:8][C:4]=2[CH:3]=1

参加物

5

反応物 4

HCID 7302Gamma-ButyrolactoneHCID 24758Sodium hydrideHCID 119541287-Chloro-2-dibenzofuranolHCID 178418361HCID 178418361、化合物

生成物 1

HCID 70588848HCID 70588848、化合物

反応条件

温度
120 °C

実験手順

110 g (0.5 mole) 7-Chloro-2-hydroxydibenzofuran is dissolved in 200 g (2.3 mole) of butyrolactone. To this solution is added 27.5 g (0.57 mole) sodium hydride 50% dispersion in oil (prewashed with petroleum ether) in small increments. When hydrogen evolution ceases the solution is heated to 120° C. for 2 hours. The excess butyrolactone was distilled off under high vacuum. The crude product was dissolved in water and precipitated into dilute acid. The product was filtered and redissolved in sodium bicarbonate solution. The solution was charcoal treated and precipitated in dilute acid filtered and dried. 137 g., m.p. 143°-145° C. were obtained. This Example corresponds to Example 69 in Table I.

後処理

  1. distillationThe excess butyrolactone was distilled off under high vacuum
  2. dissolutionThe crude product was dissolved in water
  3. customprecipitated
  4. additioninto dilute acid
  5. filtrationThe product was filtered
  6. dissolutionredissolved in sodium bicarbonate solution
  7. additiontreated
  8. customprecipitated in dilute acid
  9. filtrationfiltered
  10. customdried
  11. custom, m.p. 143°-145° C. were obtained

出典と根拠

ORDレコード
ord-ccb495ce9ea84e39b3a7e43de3f8a3b4
出典データセット
uspto-grants-1980_04
特許番号
US04199346

反応ノート

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