Pyridine → HCID 14438699, 화합물

HRID 1762781노트

반응식

HRID 1762781 반응식
[N:1]([CH2:8][CH2:9][OH:10])([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].N1C=CC=CC=1.Cl[C:18]([C:20]1[C:32]2[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:25](=[C:33]([C:36]#[N:37])[C:34]#[N:35])[C:24]=2[CH:23]=[CH:22][CH:21]=1)=[O:19]>ClCCl>[C:36]([C:33]([C:34]#[N:35])=[C:25]1[C:24]2[CH:23]=[CH:22][CH:21]=[C:20]([C:18]([O:4][CH2:3][CH2:2][N:1]([CH2:8][CH2:9][OH:10])[CH2:5][CH2:6][OH:7])=[O:19])[C:32]=2[C:31]2[C:26]1=[CH:27][CH:28]=[CH:29][CH:30]=2)#[N:37]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7618TriethanolamineHCID 198332559-(Dicyanomethylidene)-9H-fluorene-4-carbonyl chloride

생성물 1

HCID 14438699HCID 14438699, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 100.0 grams of triethanolamine and 58 milliliters of dry pyridine in 350 milliliters of dry 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 dry dichloromethane was added over a period of 1 hour. After addition, the reaction mixture was further stirred for another hour. The reaction mixture was washed several times with water to remove the excess amines and the corresponding hydrochloride salts, dried with anhydrous magnesium sulfate and filtered. Evaporation of the filtrate gave 5 grams of crude product. Purification by recrystallization from isopropanol afforded 4.5 grams of pure (1c), mp., 155.5°-156.5° C.

후처리

  1. additionAfter addition
  2. washThe reaction mixture was washed several times with water
  3. customto remove the excess amines
  4. dry with materialthe corresponding hydrochloride salts, dried with anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customEvaporation of the filtrate
  7. customgave 5 grams of crude product
  8. customPurification
  9. customby recrystallization from isopropanol

출처 및 근거

ORD 기록
ord-9b8399d3cc134ac78069fbfb0fbd8d50
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835081

반응 노트

불러오는 중…