Hydrochloric Acid → Methyl 5-(methylsulfonyl)-1H-indole-2-carboxylate

HRID 1432249

反応式

HRID 1432249 の反応式
[CH3:1][O:2][C:3]([C:5]1[N:6](S(C2C=CC=CC=2)(=O)=O)[C:7]2[C:12]([CH:13]=1)=[CH:11][C:10]([S:14]([CH3:17])(=[O:16])=[O:15])=[CH:9][CH:8]=2)=[O:4].O1CCCC1.[OH-].[K+].Cl>CO>[CH3:1][O:2][C:3]([C:5]1[NH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][C:10]([S:14]([CH3:17])(=[O:16])=[O:15])=[CH:9][CH:8]=2)=[O:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14797Potassium HydroxideHCID 684443721-Benzenesulfonyl-5-methanesulfonylindole-2-carboxylic acid methyl ester

生成物 1

HCID 735868Methyl 5-(methylsulfonyl)-1H-indole-2-carboxylate収率 97.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a mixture of the resulting 1-benzenesulfonyl-5-methanesulfonylindole-2-carboxylic acid methyl ester (3.5 g), tetrahydrofuran (45 ml) and methanol (12 ml), potassium hydroxide (0.79 g) was added at 0° C. and the mixture was stirred at the same temperature for 3 hours. 2N, hydrochloric acid was added, and the mixture was extracted with dichloromethane. The organic layer was washed with water and dried over sodium sulfate. The solvent was distilled off under reduced pressure to obtain 2.2 g of a white amorphous 5methanesulfonylindole-2-carboxylic acid methyl ester as a crude product.

後処理

  1. additionwas added at 0° C.
  2. extractionthe mixture was extracted with dichloromethane
  3. washThe organic layer was washed with water
  4. dry with materialdried over sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-3e06c91d59f744ecbfdea23701b1b44c
出典データセット
uspto-grants-2009_11
特許番号
US07612070B2

関連ノート

読み込み中…