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

HRID 1432252ノート

反応式

HRID 1432252 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e3fc24522e4740399b4932892df3af51
出典データセット
uspto-grants-2009_11
特許番号
US07612070B2

反応ノート

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