Ammonia → 1-(4-Fluorobenzyl)-5-methanesulfonylindole-2-carboxamide

HRID 1814099

반응식

HRID 1814099 반응식
[F:1][C:2]1[CH:24]=[CH:23][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][C:12]([S:16]([CH3:19])(=[O:18])=[O:17])=[CH:13][CH:14]=3)[CH:9]=[C:8]2[C:20](O)=[O:21])=[CH:4][CH:3]=1.O1CCCC1.C(Cl)(=O)OCC.[NH3:36]>O.C(N(CC)CC)C>[F:1][C:2]1[CH:24]=[CH:23][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][C:12]([S:16]([CH3:19])(=[O:18])=[O:17])=[CH:13][CH:14]=3)[CH:9]=[C:8]2[C:20]([NH2:36])=[O:21])=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 8028TetrahydrofuranHCID 10928Ethyl chloroformateHCID 225044521-(4-fluorobenzyl)-5-methanesulfonylindole-2-carboxylic Acid

생성물 1

HCID 225043691-(4-Fluorobenzyl)-5-methanesulfonylindole-2-carboxamide

시약·촉매·용매 2

HCID 962Water용매HCID 8471Triethylamine용매

실험 절차

To a mixture of the compound obtained in Example 22 (4) (0.23 g) and tetrahydrofuran (7 ml), triethylamine (0.19 ml) and ethyl chlorocarbonate (0.1 ml) were added at 0° C. and the mixture was stirred at the same temperature for 20 minutes. An ammonia gas was blown into the mixture at 0° C. and the mixture was stirred at the same temperature for 30 minutes. Water was added thereto and the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over sodium sulfate and concentrated under reduced pressure. The resulting residue was recrystallized (ethyl acetate) to obtain 0.06 g of the desired product as a white crystal.

후처리

  1. additionwere added at 0° C.
  2. customwas blown into the mixture at 0° C.
  3. stirringthe mixture was stirred at the same temperature for 30 minutes
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe resulting residue was recrystallized (ethyl acetate)

출처 및 근거

ORD 기록
ord-078af033a05e40ef886904d72cdff349
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06875770B2

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