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

HRID 1609262노트

반응식

HRID 1609262 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-62a6fc14b4454eabab8b7a3ef86e6f23
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05399703

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