Water → HCID 22123630, 화합물

HRID 1859303노트

반응식

HRID 1859303 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2([OH:38])[C:19]3[CH:20]=[CH:21][C:22]([O:24][CH2:25][O:26][CH3:27])=[CH:23][C:18]=3[O:17][CH2:16][CH:15]2[C:28]2[CH:33]=[CH:32][C:31]([O:34][CH2:35][O:36][CH3:37])=[CH:30][CH:29]=2)=[CH:10][CH:9]=1.[I-:39].[Na+].O>C(C(C)=O)C>[OH:38][C:14]1([C:11]2[CH:12]=[CH:13][C:8]([O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][I:39])=[CH:9][CH:10]=2)[C:19]2[CH:20]=[CH:21][C:22]([O:24][CH2:25][O:26][CH3:27])=[CH:23][C:18]=2[O:17][CH2:16][CH:15]1[C:28]1[CH:33]=[CH:32][C:31]([O:34][CH2:35][O:36][CH3:37])=[CH:30][CH:29]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 5238Sodium IodideHCID 22123596HCID 22123596, 화합물

생성물 1

HCID 22123630HCID 22123630, 화합물수율 75%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

4-[4-(5-Chloropentyloxy)phenyl]-4-hydroxy-7-methoxymethyloxy-3-[4-(methoxymethyloxy)phenyl]-2,3-dihydro-4H-benzopyran (167 mg, 0.3 mmol) and sodium iodide (139 mg, 0.9 mmol) were dissolved in methyl ethyl ketone (5 ml) and then refluxed for 12 hours. The reaction solution was cooled to room temperature and, after adding water, extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure to remove the organic solvent. The concentrate was subjected to column chromatography (n-hexane:ethyl acetate=4:1) to obtain 142 mg (yield: 75%) of the title compound as a colorless oil.

후처리

  1. temperaturerefluxed for 12 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customto remove the organic solvent

출처 및 근거

ORD 기록
ord-6dd27313323f43639eeb222241da25fa
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06153768

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