Water → HCID 20222067、化合物

HRID 980123ノート

反応式

HRID 980123 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 20222067HCID 20222067、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-5dbe7fa807994653afa3cb482d6162ca
出典データセット
uspto-grants-1987_01
特許番号
US04636456

反応ノート

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