Sodium Hydroxide → 3-[[[2-(Methylamino)-2-oxoethyl]amino]carbonyl]-5-nitrobenzoic acid

HRID 1606660

反応式

HRID 1606660 の反応式
[CH3:1][NH:2][C:3](=[O:21])[CH2:4][NH:5][C:6](=[O:20])[C:7]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[C:9]([C:16]([O:18]C)=[O:17])[CH:8]=1.O1CCOCC1.[OH-].[Na+]>O>[CH3:1][NH:2][C:3](=[O:21])[CH2:4][NH:5][C:6](=[O:20])[C:7]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[C:9]([C:16]([OH:18])=[O:17])[CH:8]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 312751,4-DioxaneHCID 214272733-Metoxycarbonyl-5-nitrobenzoyl-glycine methylamide

生成物 1

HCID 30164953-[[[2-(Methylamino)-2-oxoethyl]amino]carbonyl]-5-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

443.0 g. (1.5 moles) of N-(3-metoxycarbonyl-5-nitrobenzoyl-glycine methylamide in 5.5 l. of dioxane is agitated for 2 hours at room temperature with the addition of 3.3 l. of 0.5N sodium hydroxide solution. Thereafter, 400 ml. of water is added to the reaction mixture, the dioxane is distilled off under vacuum, and the acid is precipitated with concentrated hydrochloric acid, vacuum-filtered, washed free of salt with water, and dried under vacuum at 70° C. Yield: 408 g. M.P. 256- 257°C.

後処理

  1. distillationthe dioxane is distilled off under vacuum
  2. customthe acid is precipitated with concentrated hydrochloric acid
  3. filtrationvacuum-filtered
  4. washwashed free of salt with water
  5. customdried under vacuum at 70° C

出典と根拠

ORDレコード
ord-cb64c463bc614f119a91f08de97a248f
出典データセット
uspto-grants-1976_04
特許番号
US03953501

関連ノート

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