Ammonia → 2-[3-(2-Nitrophenoxy)phenoxy]propionamide

HRID 1609262ノート

反応式

HRID 1609262 の反応式
[N+:1]([C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[O:6][C:7]1[CH:8]=[C:9]([CH:16]=[CH:17][CH:18]=1)[O:10][CH:11]([CH3:15])[C:12](O)=[O:13])([O-:3])=[O:2].C([N:25](CC)CC)C.ClC(OCC)=O.N>C(Cl)Cl>[N+:1]([C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[O:6][C:7]1[CH:8]=[C:9]([CH:16]=[CH:17][CH:18]=1)[O:10][CH:11]([CH3:15])[C:12]([NH2:25])=[O:13])([O-:3])=[O:2]

参加物

6

反応物 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 200844942-[3-(2-Nitrophenoxy)phenoxy]propionic acid

生成物 1

HCID 200843872-[3-(2-Nitrophenoxy)phenoxy]propionamide収率 53.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In 100 ml of methylene chloride were dissolved 6.15 g of 2-[3-(2-nitrophenoxy)phenoxy]propionic acid and 4.2 g of triethylamine, followed by dropwise addition of 2.5 g of ethyl chloroformate at a temperature not exceeding 0° C., and the mixture was further stirred at the same temperature for 30 minutes. The reaction mixture was poured into previously ice-cooled methylene chloride (120 ml) saturated with ammonia gas and the mixture was then stirred at room temperature for 30 minutes. The methylene chloride layer was washed with water (twice), dried and concentrated and the residue was crystallized from methanol and isopropyl ether to give 3.3 g of the title compound.

後処理

  1. customexceeding 0° C.
  2. additionThe reaction mixture was poured into previously ice-
  3. stirringthe mixture was then stirred at room temperature for 30 minutes
  4. washThe methylene chloride layer was washed with water (twice),
  5. customdried
  6. concentrationconcentrated
  7. customthe residue was crystallized from methanol and isopropyl ether

出典と根拠

ORDレコード
ord-62a6fc14b4454eabab8b7a3ef86e6f23
出典データセット
uspto-grants-1995_03
特許番号
US05399703

反応ノート

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