Sulfuryl chloride → Methyl 3-chloro-4,5-dihydroxybenzoate

HRID 1512777노트

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HRID 1512777 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[OH:12])[C:5]([O:7][CH3:8])=[O:6].S(Cl)([Cl:16])(=O)=O>C(OCC)C>[Cl:16][C:10]1[CH:9]=[C:4]([CH:3]=[C:2]([OH:1])[C:11]=1[OH:12])[C:5]([O:7][CH3:8])=[O:6]

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 287064Methyl 3,4-Dihydroxybenzoate

생성물 1

HCID 21649010Methyl 3-chloro-4,5-dihydroxybenzoate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
0 °C

실험 절차

To a suspension of methyl 3,4-dihydroxybenzoate (5.0 g) in diethyl ether (300 mL) stirred at 0° C. was added sulfuryl chloride (3.7 mL) dropwise. The reaction mixture was stirred at 0° C. for 16 h. The solvent was removed in vacuo. The residue was washed with hot chloroform (2×150 mL) to afford methyl 3-chloro-4,5-dihydroxybenzoate (D68) (1.9 g) as a white solid. δH (DMSO-d6, 400 MHz): 3.78 (3H, s), 7.33 (1H, d), 7.37 (1H, d), 10.11 (2H, br s). MS (ES): C8H7ClO4 requires 202. found 203.0 (M+H+).

후처리

  1. stirringThe reaction mixture was stirred at 0° C. for 16 h
  2. customThe solvent was removed in vacuo
  3. washThe residue was washed with hot chloroform (2×150 mL)

출처 및 근거

ORD 기록
ord-5c538f6a57c2464da7cd0d541dfa27ff
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217028B2

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