Methylamine → HCID 20071071、化合物

HRID 2291439ノート

反応式

HRID 2291439 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4](Cl)[C:3]=1[N+:10]([O-:12])=[O:11].CN.ClC1C=[C:20]([NH:22]C)C([N+]([O-])=O)=C(NC)C=1>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH:22][CH3:20])[C:3]=1[N+:10]([O-:12])=[O:11]

参加物

5

反応物 3

HCID 6329MethylamineHCID 292282,4,6-TrichloronitrobenzeneHCID 20071079HCID 20071079、化合物

生成物 1

HCID 20071071HCID 20071071、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.150 mole (34 g) of 2,4,6-trichloronitrobenzene is added portionwise, at ambient temperature, to 300 ml of a 30% strength solution of methylamine in absolute ethanol. After stirring for 23 hours at ambient temperature, a precipitate, consisting essentially of 4-chloro-2-methylamino-6-methylaminonitrobenzene, is removed by filtration. The filtrate is evaported to dryness under reduced pressure. 800 ml of concentrated hydrochloric acid are added to the dry extract obtained in this manner. The insoluble fraction is removed by filtration. After dilution of the filtrate with 650 ml of water, the expected product precipitates. It is washed with water and is then dried under vacuum in the presence of phosphorus pentoxide. After recrystallization from isopropanol and then from absolute ethanol, it melts at 120° C.

後処理

  1. customis removed by filtration
  2. addition800 ml of concentrated hydrochloric acid are added to the dry
  3. extractionextract
  4. customobtained in this manner
  5. customThe insoluble fraction is removed by filtration
  6. customAfter dilution of the filtrate with 650 ml of water, the expected product precipitates
  7. washIt is washed with water
  8. dry with materialis then dried under vacuum in the presence of phosphorus pentoxide
  9. customAfter recrystallization from isopropanol

出典と根拠

ORDレコード
ord-c38195ce70ed44fd8bb62dd21748faff
出典データセット
uspto-grants-1989_01
特許番号
US04797129

反応ノート

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