4-Chloro-N-methylbenzenamine → Hydrochloric Acid

HRID 358035

反応式

HRID 358035 の反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([Cl:12])=[CH:9][CH:10]=2)[N:5]=[CH:4][N:3]=1.[Cl:13][C:14]1[CH:21]=[CH:20][C:17]([NH:18][CH3:19])=[CH:16][CH:15]=1>C(O)C>[Cl:12][C:8]1[CH:7]=[C:6]2[C:11]([C:2]([N:18]([CH3:19])[C:17]3[CH:20]=[CH:21][C:14]([Cl:13])=[CH:15][CH:16]=3)=[N:3][CH:4]=[N:5]2)=[CH:10][CH:9]=1.[ClH:1]

参加物

5

反応物 2

HCID 702724-Chloro-N-methylbenzenamineHCID 2418814,7-Dichloroquinazoline

生成物 2

HCID 313Hydrochloric AcidHCID 127745177-Chloro-4-(4'-chloro-N-methylanilino)quinazoline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2.5 g of 4,7-dichloroquinazoline and 2.2 g of p-chloro-N-methylaniline were added to 10 ml of ethanol and then the mixture was heated. The mixture became a homogeneous solution which solidified soon after. After cooling, the solidified crystals were collected and recrystallized from ethanol to give the desired compound in the form of its hydrochloride (Compound No. 68). The crystals of hydrochloride were crushed and added to a dilute aqueous solution of sodium hydroxide, with stirring, to precipitate the free base. The precipitate was collected by filtration, washed with water and recrystallized from ethanol to give 2.4 g (yield 65%) of the desired Compound No. 67 in the form of colourless plates melting at 129°-131° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureAfter cooling
  3. customthe solidified crystals were collected
  4. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-eb6788864d8246b19c761fdf5d1dd535
出典データセット
uspto-grants-1984_08
特許番号
US04464375

関連ノート

読み込み中…