Dimethyl Sulfate → HCID 18986212, 화합물

HRID 2396825노트

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HRID 2396825 반응식
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([F:13])=[CH:10][CH:11]=2)[C:6](=[O:14])[CH2:5]1)(=[O:3])[CH3:2].[OH-].[Na+].S(OC)(O[CH3:21])(=O)=O>C(=O)(O)[O-].[Na+]>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([F:13])=[CH:10][CH:11]=2)[C:6]([O:14][CH3:21])=[CH:5]1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 189863261-Acetyl-5-fluoro-1,2-dihydro-3H-indol-3-one

생성물 1

HCID 18986212HCID 18986212, 화합물수율 86%

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

실험 절차

A mixture of 1.6 g of 1-acetyl-5-fluoroindolin-3-one, 1.9 g of powdered sodium hydroxide and 28 ml of dimethyl sulfate was stirred at room temperature for two hours. After the addition of 240 ml of saturated sodium bicarbonate solution the mixture was stirred overnight and subsequently filtered. The residue was taken up in 100 ml of ether and 100 ml of ethyl acetate. The solution was dried over sodium sulfate, filtered and evaporated. There were obtained 1.47 g (86%) of 1-acetyl-5-fluoro-3-methoxyindole as greenish crystals with m.p. 124°-125°.

후처리

  1. stirringwas stirred overnight
  2. filtrationsubsequently filtered
  3. dry with materialThe solution was dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-d458808d652b46499f344d6e802f1ed4
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05494928

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