Sodium Hydroxide → Tucaresol

HRID 485181

反応式

HRID 485181 の反応式
[CH:1]([C:3]1[C:21]([OH:22])=[CH:20][CH:19]=[CH:18][C:4]=1[O:5][CH2:6][C:7]1[CH:17]=[CH:16][C:10]([C:11]([O:13]CC)=[O:12])=[CH:9][CH:8]=1)=[O:2].[OH-].[Na+]>CO>[CH:1]([C:3]1[C:21]([OH:22])=[CH:20][CH:19]=[CH:18][C:4]=1[O:5][CH2:6][C:7]1[CH:17]=[CH:16][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1)=[O:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 9861133Ethyl 4-(2-formyl-3-hydroxyphenoxymethyl)benzoate

生成物 1

HCID 55223Tucaresol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The product from step (B) (7.9 g) was suspended in methanol (90 ml) and stirred with 1 N sodium hydroxide solution (90 ml) for 2.5 hours. The resulting dark solution was evaporated to half volume and then diluted with water (160 ml) and acidified with concentrated hydrochloric acid, with cooling in an ice bath. The precipitated product was collected by filtration, washed with water (200 ml), sucked dry and recrystallised from aqueous dimethylformamide. The title compound was isolated as yellow crystals after drying in vacuo at 60° C. m.p. 240°-242° C. (sinters at ~225° C.)

後処理

  1. customThe resulting dark solution was evaporated to half volume
  2. additiondiluted with water (160 ml)
  3. temperaturewith cooling in an ice bath
  4. filtrationThe precipitated product was collected by filtration
  5. washwashed with water (200 ml)
  6. customsucked dry
  7. customrecrystallised from aqueous dimethylformamide

出典と根拠

ORDレコード
ord-d392710462df4f4faf857a804d97a8c4
出典データセット
uspto-grants-1985_08
特許番号
US04535183

関連ノート

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