Sodium Hydroxide → Tucaresol

HRID 485181

반응식

HRID 485181 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 55223Tucaresol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.)

후처리

  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

출처 및 근거

ORD 기록
ord-d392710462df4f4faf857a804d97a8c4
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04535183

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