Pyrogallol → Bendiocarb phenol

HRID 1438811ノート

反応式

HRID 1438811 の反応式
[C:1]1([CH:9]=[CH:8][CH:7]=[C:5]([OH:6])[C:3]=1[OH:4])[OH:2].[C:10]1(C)[C:11](S(O)(=O)=O)=CC=C[CH:15]=1>COC(OC)(C)C.C1C=CC=CC=1>[OH:2][C:1]1[C:3]2[O:4][C:10]([CH3:11])([CH3:15])[O:6][C:5]=2[CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 2

HCID 1057PyrogallolHCID 69252-Methylbenzenesulfonic acid

生成物 1

HCID 62765Bendiocarb phenol

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 64952,2-Dimethoxypropane溶媒

実験手順

A solution of pyrogallol (63 parts) in 2,2-dimethoxypropane (100 parts) and benzene (100 parts) containing toluenesulphonic acid (0.01 parts) was slowly distilled through a fractionating column during 4 hours, removing liquid (150 parts), boiling point 57°-64° C. A few drops of triethylamine were then added and the mixture thoroughly washed with water, dried and evaporated. Distillation gave 4-hydroxy-2,2-dimethyl-1,3-benzodioxole (36 parts), boiling point 110° C/0.7 mm., which was purified by recrystallisation from carbon tetrachloride. Melting point 88°-90° C.

後処理

  1. distillationwas slowly distilled through a fractionating column during 4 hours
  2. customremoving liquid (150 parts), boiling point 57°-64° C
  3. additionA few drops of triethylamine were then added
  4. washthe mixture thoroughly washed with water
  5. customdried
  6. customevaporated
  7. distillationDistillation

出典と根拠

ORDレコード
ord-734d5d7b0c1b450eac8d7268ccb9b696
出典データセット
uspto-grants-1977_11
特許番号
US04056625

反応ノート

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