Hydrochloric Acid → 2-(4-Hydroxyphenylthio)-7-isopropoxy-5-methoxychromone

HRID 441061노트

반응식

HRID 441061 반응식
[CH:1]([O:4][C:5]1[CH:14]=[C:13]2[C:8]([C:9](=[O:18])[CH:10]=[C:11]([S:15]([CH3:17])=O)[O:12]2)=[C:7]([O:19][CH3:20])[CH:6]=1)([CH3:3])[CH3:2].[OH:21][C:22]1[CH:27]=[CH:26]C(S)=[CH:24][CH:23]=1.C(=O)([O-])[O-].[K+].[K+].Cl>CC(C)=O>[OH:21][C:22]1[CH:27]=[CH:26][C:17]([S:15][C:11]2[O:12][C:13]3[C:8]([C:9](=[O:18])[CH:10]=2)=[C:7]([O:19][CH3:20])[CH:6]=[C:5]([O:4][CH:1]([CH3:3])[CH3:2])[CH:14]=3)=[CH:24][CH:23]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 2401474-MercaptophenolHCID 229064677-Isopropoxy-5-methoxy-2-methylsulfinylchromone

생성물 1

HCID 229064892-(4-Hydroxyphenylthio)-7-isopropoxy-5-methoxychromone수율 57.7%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 146 mg of 7-isopropoxy-5-methoxy-2-methylsulfinylchromone (0.493 mmol ) , 93 mg of 4-hydroxybenzenethiol(0.740 mmol), 102 mg of potassium carbonate (0.740 mmol) and 6 ml acetone was stirred for 2 hours at room temperature. The reaction solution was neutralized with dilute hydrochloric acid and extracted twice with ethyl acetate, and the organic layer was washed with saturated NaCl water and was then dried over sodium sulfate anhydride. The solvent was distilled off under reduced pressure, and the crude product was subjected to recrystallization from acetone-methanol, to give 102 mg of 2-(4-hydroxyphenylthio)-7-isopropoxy-5-methoxychromone (57% yield).

후처리

  1. extractionextracted twice with ethyl acetate
  2. washthe organic layer was washed with saturated NaCl water
  3. dry with materialwas then dried over sodium sulfate anhydride
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe crude product was subjected to recrystallization from acetone-methanol

출처 및 근거

ORD 기록
ord-b75679b73f6449178d2300d616707cb5
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521216

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