N-Carbethoxyphthalimide → 4-(2-Nitrophenyl)-2-phthalimidobutyric acid

HRID 1194974ノート

反応式

HRID 1194974 の反応式
[NH2:1][CH:2]([CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[N+:14]([O-:16])=[O:15])[C:3]([OH:5])=[O:4].C(OC(N1[C:26](=[O:27])[C:25]2=[CH:28][CH:29]=[CH:30][CH:31]=[C:24]2[C:23]1=[O:32])=O)C>C(=O)([O-])[O-].[Na+].[Na+]>[N+:14]([C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[CH2:7][CH2:6][CH:2]([N:1]1[C:26](=[O:27])[C:25]2=[CH:28][CH:29]=[CH:30][CH:31]=[C:24]2[C:23]1=[O:32])[C:3]([OH:5])=[O:4])([O-:16])=[O:15]

参加物

4

反応物 2

HCID 31187N-CarbethoxyphthalimideHCID 132435482-Amino-4-(2-nitrophenyl)butyric acid

生成物 1

HCID 144072514-(2-Nitrophenyl)-2-phthalimidobutyric acid収率 70.3%

試薬・触媒・溶媒 1

HCID 10340Sodium Carbonate溶媒

実験手順

In an aqueous solution (150 ml) of 6.1 g of sodium carbonate is dissolved 11.7 g of 2-amino-4-(2-nitrophenyl)butyric acid, and 15 g of N-ethoxycarbonylphthalimide is added to the solution under stirring. After stirring at room temperature overnight, the insoluble material is removed by filtration, and the filtrate is made weakly acidic with concentrated hydrochloric acid. The viscous material, which separates out, is admixed with 50 ml of ethanol, followed by stirring, whereby there separate out crystals. The crystals are collected by filtration and dried to give 13 g of 4-(2-nitrophenyl)-2-phtalimidobutyric acid as colorless crystals. m.p. 177°-179° C.

後処理

  1. additionis added to the solution
  2. stirringAfter stirring at room temperature overnight
  3. customthe insoluble material is removed by filtration
  4. stirringby stirring
  5. customwhereby there separate out crystals
  6. filtrationThe crystals are collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-f10ab8cfddd64e9799ef9157aef9beda
出典データセット
uspto-grants-1989_03
特許番号
US04816466

反応ノート

読み込み中…