Dimethyl Sulfate → HCID 18986212、化合物

HRID 2396825ノート

反応式

HRID 2396825 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 18986212HCID 18986212、化合物収率 86%

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

実験手順

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°.

後処理

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

出典と根拠

ORDレコード
ord-d458808d652b46499f344d6e802f1ed4
出典データセット
uspto-grants-1996_02
特許番号
US05494928

反応ノート

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