Formic Acid → N,N-Dimethyl-2-aminosulfonyl-4-formamidobenzamide

HRID 505949

反応式

HRID 505949 の反応式
[CH3:1][N:2]([CH3:18])[C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-])=O)=[CH:6][C:5]=1[S:13]([NH2:16])(=[O:15])=[O:14].[CH:19](O)=[O:20]>[O-][Mo]([O-])(=O)=O.[Na+].[Na+].[Pd]>[CH3:1][N:2]([CH3:18])[C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][CH:19]=[O:20])=[CH:6][C:5]=1[S:13]([NH2:16])(=[O:15])=[O:14]

参加物

5

反応物 2

HCID 284Formic AcidHCID 22066001N,N-Dimethyl-4-nitro-2-sulfamoylbenzamide

生成物 1

HCID 15240549N,N-Dimethyl-2-aminosulfonyl-4-formamidobenzamide

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 61424Sodium Molybdate触媒

反応条件

温度
20 °C

実験手順

A suspension of 40 g N,N-Dimethyl 2-aminosulfonyl-4-nitrobenzamide (VIII), sodium molybdate (0.08 g) and Pd/C (3 g, 5%, 50% water) in formic acid (200 ml) was hydrogenated at 50° C. and 40 bar for 7 hours. The catalyst was then filtered and washed with formic acid (20 ml). The filtrate was concentrated in vacuo and ethyl acetate (200 ml) added. After stirring for 2 hours at 20° C. the product was filtered, the filtrate concentrated and re-filtered. The combined solids were washed with ethyl acetate (20 ml) and dries at 50° C./50 mbar. Yield: 35.3 g (=84.3%), 94.1% w/w, mp.: 192-193° C.

後処理

  1. customwas hydrogenated at 50° C.
  2. filtrationThe catalyst was then filtered
  3. washwashed with formic acid (20 ml)
  4. concentrationThe filtrate was concentrated in vacuo and ethyl acetate (200 ml)
  5. additionadded
  6. filtrationwas filtered
  7. concentrationthe filtrate concentrated
  8. filtrationre-filtered
  9. washThe combined solids were washed with ethyl acetate (20 ml) and dries at 50° C./50 mbar

出典と根拠

ORDレコード
ord-2859279ccf80494dbc0d185f567de2f3
出典データセット
uspto-grants-2010_08
特許番号
US07781611B2

関連ノート

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