4-Methyl-5-nitrosaccharin → 4-Methyl-5-aminosaccharin

HRID 809

反応式

HRID 809 の反応式
[CH3:1][C:2]1[C:12]([N+:13]([O-])=O)=[CH:11][CH:10]=[C:9]2[C:3]=1[C:4](=[O:16])[NH:5][S:6]2(=[O:8])=[O:7].[H][H]>O.[Pd]>[CH3:1][C:2]1[C:12]([NH2:13])=[CH:11][CH:10]=[C:9]2[C:3]=1[C:4](=[O:16])[NH:5][S:6]2(=[O:8])=[O:7]

参加物

5

反応物 2

HCID 153345344-Methyl-5-nitrosaccharinHCID 178418361HCID 178418361、化合物

生成物 1

HCID 701876914-Methyl-5-aminosaccharin

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

反応条件

温度
45 °C

実験手順

33.6 g (0.13 mol) of 4-methyl-5-nitrosaccharin are dissolved in 1.2 l of water with warming to 45° C. and 5 g of Pd/C (10% on active carbon) are added. Hydrogen gas is then passed in with vigorous stirring (pressureless hydrogenation). 9 l of H2 are absorbed in the course of 4.5 hours. After cooling to 25° C., the catalyst is filtered off, and the filtrate is concentrated to a volume of 200 ml and then acidified to pH 1. The deposited precipitate is filtered off with suction, washed with water and dried under reduced pressure at 50° C. 23.4 g (0.11 mol=85% of theory) of a white solid of m.p.: 272°-273° C. are obtained.

後処理

  1. custom9 l of H2 are absorbed in the course of 4.5 hours
  2. temperatureAfter cooling to 25° C.
  3. filtrationthe catalyst is filtered off
  4. concentrationthe filtrate is concentrated to a volume of 200 ml
  5. filtrationThe deposited precipitate is filtered off with suction
  6. washwashed with water
  7. customdried under reduced pressure at 50° C
  8. custom23.4 g (0.11 mol=85% of theory) of a white solid of m.p.: 272°-273° C. are obtained

出典と根拠

ORDレコード
ord-67ec3bcdf85a4cd095b46cc07afa68ed
出典データセット
uspto-grants-1998_03
特許番号
US05723415

関連ノート

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