4-Chloro-N-methylbenzenamine → Hydrochloric Acid

HRID 358035

반응식

HRID 358035 반응식
[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]

참가 물질

5

반응물 2

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

생성물 2

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-eb6788864d8246b19c761fdf5d1dd535
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04464375

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