Acetic Anhydride → HCID 21401618, 화합물

HRID 973199노트

반응식

HRID 973199 반응식
[OH:1][CH:2]([CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=1)[CH2:3][CH2:4][CH2:5][NH:6][S:7]([CH3:10])(=[O:9])=[O:8].C([O:23][C:24](=[O:26])[CH3:25])(=O)C>C(OCC)C>[C:2]([O:1][CH:2]([CH2:11][O:12][C:13]1[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=1)[CH2:3][CH2:4][CH2:5][N:6]([CH2:15][CH2:14][CH2:13][CH2:18][CH2:17][CH2:25][C:24]([OH:23])=[O:26])[S:7]([CH3:10])(=[O:9])=[O:8])(=[O:1])[CH3:3]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 86735163N-[4-Hydroxy-5-(4-fluorophenoxy)pentyl]-methanesulfonamide

생성물 1

HCID 21401618HCID 21401618, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 7-{N-[4-hydroxy-45-(4-fluorophenoxy)- pentyl]methanesulfonamido}heptanoic acid (12.3 g., 0.03 mole) (Example 1, Step E) and acetic anhydride (6.1 g., 0.06 mole) is kept at room temperature for 18 hours. This mixture is taken up in 80 ml. of ethyl ether. The solution is extracted with an ice-cold solution of 8 g. of sodium hydroxide in 150 ml. of water. The basic solution is separated and acidified with concentrated hydrochloric acid. The crude product that separates is extracted into ether, washed with water and dried over sodium sulfate. The ether is evaporated and the residual oil is purified by chromatography on silica gel using 2% methanol in chloroform as the eluting solvent. There is obtained 7-{N-[4- acetoxy-5-(4-fluorophenoxy)pentyl]methanesulfonamido}- heptanoic acid as a viscous oil.

후처리

  1. extractionThe solution is extracted with an ice-cold solution of 8 g
  2. customThe basic solution is separated
  3. extractionThe crude product that separates is extracted into ether
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customThe ether is evaporated
  7. customthe residual oil is purified by chromatography on silica gel using 2% methanol in chloroform as the eluting solvent

출처 및 근거

ORD 기록
ord-38c1fdb879ac43e9a0c3bb65961a26c9
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04055596

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