Hydrochloric Acid → 2-Carbamoyl-6-nitrobenzoic Acid

HRID 1193012

反応式

HRID 1193012 の反応式
[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:7]([NH:9][C:10](=[O:11])[C:5]=12)=[O:8])([O-:3])=[O:2].[OH-:15].[Na+].Cl>O>[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]([C:7]([NH2:9])=[O:8])[C:5]=1[C:10]([OH:15])=[O:11])([O-:3])=[O:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 117793-NitrophthalimideHCID 14798Sodium Hydroxide

生成物 1

HCID 45927482-Carbamoyl-6-nitrobenzoic Acid収率 73%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
5 °C

実験手順

A suspension of 57.6 g of 3-nitro-phthalimide (0.3 mol) in 672 g of water is cooled to 5° C. 80 g of 30% sodium hydroxide solution (0.6 mol, 2 equivalents) are added in the shortest possible time. After 2 hours at 5° C., the reaction mixture is added at 5° C. to 65 g of 32% hydrochloric acid solution (0.57 mol, 1.9 equivalents), which is diluted beforehand with 72 ml of water. The pH value is adjusted to 2-2.5 and the crude product which crystallises out is filtered off and washed twice with water. 6-Nitrophthalamic acid is obtained in a yield of 73%.

後処理

  1. customthe crude product which crystallises out
  2. filtrationis filtered off
  3. washwashed twice with water

出典と根拠

ORDレコード
ord-b974181caabc42a29878846970d982df
出典データセット
uspto-grants-2014_03
特許番号
US08680337B2

関連ノート

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