1-Adamantaneacetic acid → HCID 70523886, 화합물

HRID 904855노트

반응식

HRID 904855 반응식
Cl.Cl.[NH2:3][C:4]1[CH:10]=[C:9]([Cl:11])[C:8]([S:12](=[O:15])(=[O:14])[NH2:13])=[CH:7][C:5]=1[NH2:6].[C:16]12([CH2:26][C:27](O)=O)[CH2:25][CH:20]3[CH2:21][CH:22]([CH2:24][CH:18]([CH2:19]3)[CH2:17]1)[CH2:23]2>>[OH2:14].[C:16]12([CH2:26][C:27]3[NH:6][C:5]4[CH:7]=[C:8]([S:12](=[O:14])(=[O:15])[NH2:13])[C:9]([Cl:11])=[CH:10][C:4]=4[N:3]=3)[CH2:17][CH:18]3[CH2:24][CH:22]([CH2:21][CH:20]([CH2:19]3)[CH2:25]1)[CH2:23]2.[C:16]12([CH2:26][C:27]3[NH:6][C:5]4[CH:7]=[C:8]([S:12](=[O:14])(=[O:15])[NH2:13])[C:9]([Cl:11])=[CH:10][C:4]=4[N:3]=3)[CH2:17][CH:18]3[CH2:24][CH:22]([CH2:21][CH:20]([CH2:19]3)[CH2:25]1)[CH2:23]2

참가 물질

3

반응물 2

HCID 1232211-Adamantaneacetic acidHCID 20477848HCID 20477848, 화합물

생성물 1

HCID 70523886HCID 70523886, 화합물수율 35.5%

실험 절차

A mixture of 1.6 g of 2-amino-4-chloro-5-sulfamylaniline dihydrochloride and 1.6 g of 1-adamantane acetic acid was heated at 180°-200° for 5 hours. The mixture was cooled and the solid collected and ground into a fine powder; this was then added slowly to 100 ml of concentrated ammonium hydroxide with stirring. After stirring for twenty minutes, the solid was collected by filtration and then added to 150 ml of methanol, brought to a boil, charcoal added, and boiling continued for five minutes. The mixture was filtered through two sheets of filter paper, cooled, filtered through Celite, and then concentrated in vacuo to a dark pink solid. Recrystallization from acetonitrile provided 0.5 g of product, m.p. 203°-205°.

후처리

  1. temperaturewas heated at 180°-200° for 5 hours
  2. temperatureThe mixture was cooled
  3. customthe solid collected
  4. additionthis was then added slowly to 100 ml of concentrated ammonium hydroxide
  5. stirringAfter stirring for twenty minutes
  6. filtrationthe solid was collected by filtration
  7. additionadded to 150 ml of methanol
  8. additionadded
  9. filtrationThe mixture was filtered through two sheets of filter paper
  10. temperaturecooled
  11. filtrationfiltered through Celite
  12. concentrationconcentrated in vacuo to a dark pink solid
  13. customRecrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-94291372bdaa4c61b41100a9295ace6e
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04420487

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