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

HRID 26341

反応式

HRID 26341 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-feed1d7a0f434c569dd8e4f86e79b22d
出典データセット
uspto-grants-1979_04
特許番号
US04149848

関連ノート

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