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Thionyl Chloride → 6,7-Dimethoxynaphthalene-2-sulfonyl chloride

HRID 866900
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HRID 866900 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[CH:9]=[C:8]([S:15]([O-:18])(=O)=[O:16])[CH:7]=[CH:6]2.[Na+].S(Cl)([Cl:22])=O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[CH:9]=[C:8]([S:15]([Cl:22])(=[O:18])=[O:16])[CH:7]=[CH:6]2
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참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 23721231HCID 23721231, 화합물

생성물 1

HCID 144577546,7-Dimethoxynaphthalene-2-sulfonyl chloride

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred suspension of 50 g of finely divided sodium 6,7-dimethoxy-2-naphthalenesulfonate in 100 ml of dimethylformamide was added dropwise 62.2 ml of thionyl chloride at room temperature. After 30 minutes, the reaction mixture was poured into 1 l of ice water, and the precipitate filtered and then dissolved into 250 ml of benzene. The benzene solution was repeatedly washed with water and dried over anhydrous sodium sulfate. The solvent was evaporated to dryness in vacuo, and the residue was recrystallized from benzene-n-hexane (1 : 1) to give 32 g of 6,7-dimethoxy-2-naphthalenesulfonyl chloride, M.P. 127.5° - 129.5° C

후처리

  1. filtrationthe precipitate filtered
  2. dissolutiondissolved into 250 ml of benzene
  3. washThe benzene solution was repeatedly washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated to dryness in vacuo
  6. customthe residue was recrystallized from benzene-n-hexane (1 : 1)

출처 및 근거

ORD 기록
ord-22e2098687e74f1b955b4fef5757087e
출처 데이터셋
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04101653

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