1,2-Dichloro-4-nitrobenzene → 2-chloro-4-nitro-N-tetrahydrofurfurylaniline

HRID 26341

반응식

HRID 26341 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1Cl.[CH2:12]([NH2:18])[CH:13]1[O:17][CH2:16][CH2:15][CH2:14]1>O>[Cl:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[NH:18][CH2:12][CH:13]1[O:17][CH2:16][CH2:15][CH2:14]1

참가 물질

4

반응물 2

HCID 74431,2-Dichloro-4-nitrobenzeneHCID 253298Tetrahydrofurfurylamine

생성물 1

HCID 213228042-chloro-4-nitro-N-tetrahydrofurfurylaniline

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

A mixture of 0.3 mol (57.6 g) of 3,4-dichloronitrobenzene and 1 mol (101 g) of tetrahydrofurfurylamine is heated in an oil bath. When the temperature of the reaction medium reaches 110° C., the reaction starts and the temperature rises rapidly to 160° C. and is maintained for a certain time without external heating. When the temperature falls, the reaction medium is heated for 30 minutes in an oil bath at 150° C. and is then poured into 500 ml of ice-cooled water. The expected product initially precipitates in the form of an oil which rapidly crystallises. After it has been filtered off, washed with water, recrystallised and dried in vacuo, the product melts at 70° C.

후처리

  1. temperatureis heated in an oil bath
  2. custommedium reaches 110° C.
  3. customrises rapidly to 160° C.
  4. temperatureis maintained for a certain time without external heating
  5. customThe expected product initially precipitates in the form of an oil which
  6. customrapidly crystallises
  7. filtrationAfter it has been filtered off
  8. washwashed with water
  9. customrecrystallised
  10. customdried in vacuo

출처 및 근거

ORD 기록
ord-feed1d7a0f434c569dd8e4f86e79b22d
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04149848

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