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

HRID 1606660

반응식

HRID 1606660 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cb64c463bc614f119a91f08de97a248f
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03953501

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