Phloroglucinol → HCID 14438698, 화합물

HRID 1762780노트

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HRID 1762780 반응식
[C:1]1([CH:9]=[C:7]([OH:8])[CH:6]=[C:4]([OH:5])[CH:3]=1)[OH:2].N1C=CC=CC=1.Cl[C:17]([C:19]1[C:31]2[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[C:24](=[C:32]([C:35]#[N:36])[C:33]#[N:34])[C:23]=2[CH:22]=[CH:21][CH:20]=1)=[O:18]>ClCCl>[C:35]([C:32]([C:33]#[N:34])=[C:24]1[C:23]2[CH:22]=[CH:21][CH:20]=[C:19]([C:17]([O:2][C:1]3[CH:9]=[C:7]([OH:8])[CH:6]=[C:4]([OH:5])[CH:3]=3)=[O:18])[C:31]=2[C:30]2[C:25]1=[CH:26][CH:27]=[CH:28][CH:29]=2)#[N:36]

참가 물질

5

반응물 3

HCID 359PhloroglucinolHCID 1049PyridineHCID 198332559-(Dicyanomethylidene)-9H-fluorene-4-carbonyl chloride

생성물 1

HCID 14438698HCID 14438698, 화합물수율 58.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 30.0 grams of phloroglucinol and 70 milliliters of pyridine in 300 milliliters of dichloromethane was stirred at room temperature under a nitrogen atmosphere. A solution of 8.0 grams of (4-chloroformyl-9-fluorenylidene)malononitrile in 400 milliliters of dichloromethane was added over a period of 1 hour. After addition, the reaction mixture was further stirred for another hour. The mixture was washed three times with dilute aqueous HCl solution, twice with dilute aqueous NaHCO3 solution, and once with water. The solution was dried, filtered and evaporated under reduced pressure to give the crude product. Recrystallization from methanol afforded 6.1 grams of (1b), mp., 255.5°-257° C.

후처리

  1. additionAfter addition
  2. washThe mixture was washed three times with dilute aqueous HCl solution
  3. customThe solution was dried
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customto give the crude product
  7. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-95c5a72060cc4d00a8d9ef8ae0eb6a00
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835081

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