Water → HCID 20222067, 화합물

HRID 980123노트

반응식

HRID 980123 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:15]=[C:14]([OH:16])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]=1[OH:17])=[O:5])[CH3:2].S(Cl)([Cl:21])(=O)=O.O>C(Cl)(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[C:7](=[O:17])[C:8]2[C:13]([C:14](=[O:16])[C:15]=1[Cl:21])=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 24648Sulfuryl chlorideHCID 12388086Ethyl 1,4-dihydroxynaphthalene-2-carboxylate

생성물 1

HCID 20222067HCID 20222067, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

23 g of compound (6) prepared above was suspended in 300 ml of chloroform and, while keeping the solution at 5°-10° C., 27.4 g of sulfuryl chloride was slowly dropwise added thereto. After reacting for 1.5 hours, water was added to the reaction solution to conduct separation and extraction. The organic phase was dried with anhydrous sodium sulfate, and chloroform was distilled off under reduced pressure. Rapid purification of the residue through silica gel column chromatography gave compound (7) as crystals. Yield: 8.8 g (33%).

후처리

  1. customat 5°-10° C.
  2. customseparation and extraction
  3. dry with materialThe organic phase was dried with anhydrous sodium sulfate, and chloroform
  4. distillationwas distilled off under reduced pressure
  5. customRapid purification of the residue through silica gel column chromatography

출처 및 근거

ORD 기록
ord-5dbe7fa807994653afa3cb482d6162ca
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04636456

반응 노트

불러오는 중…