Water → N-[4-Hydroxy-5-(4-fluorophenoxy)pentyl]-methanesulfonamide

HRID 973191ノート

反応式

HRID 973191 の反応式
[OH:1][CH:2]([CH2:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=1)[CH2:3][CH2:4][CH2:5][N:6](CCCCCCC(OCC)=O)[S:7]([CH3:10])(=[O:9])=[O:8].[OH-].[Na+].O>C(O)C>[OH:1][CH:2]([CH2:22][O:23][C:24]1[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=1)[CH2:3][CH2:4][CH2:5][NH:6][S:7]([CH3:10])(=[O:9])=[O:8]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 21401586Ethyl 7-{N-[4-hydroxy-5-(4-fluorophenoxy)pentyl]methanesulfonamido}heptanoate

生成物 1

HCID 86735163N-[4-Hydroxy-5-(4-fluorophenoxy)pentyl]-methanesulfonamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution composed of ethyl 7-{N-[4-hydroxy-5-(4-fluorophenoxy)pentyl]methanesulfonamido}heptanoate (4.7 g., 0.11 mole), sodium hydroxide (1.0 g.), water (13 ml.) and ethanol (130 ml.) is kept at room temperature for 20 hours. Most of the solvent is removed in vacuo, water (150 ml.) is added and the solution extracted with ether (100 ml.). The aqueous layer is acidified (hydrochloric acid) and extracted with ethyl acetate (2 × 100 ml.). The organic layer is dried over sodium sulfate then concentrated in vacuo to obtain the subject compound. The yield is 3.7 g. (84%) of heavy oil.

後処理

  1. customMost of the solvent is removed in vacuo, water (150 ml.)
  2. additionis added
  3. extractionthe solution extracted with ether (100 ml.)
  4. extractionextracted with ethyl acetate (2 × 100 ml.)
  5. dry with materialThe organic layer is dried over sodium sulfate
  6. concentrationthen concentrated in vacuo
  7. customto obtain the subject compound

出典と根拠

ORDレコード
ord-8aea0f1d361d4030aa76e40050d27a5d
出典データセット
uspto-grants-1977_10
特許番号
US04055596

反応ノート

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