Toluene → 4-(4-Chloro-2-fluoroanilino)-6-methoxy-7-(2-(methylamino)ethoxy)quinazoline hydrochloride hydrate

HRID 1737552ノート

反応式

HRID 1737552 の反応式
C(O)(C(F)(F)F)=[O:2].[Cl:8][C:9]1[CH:39]=[CH:38][C:12]([NH:13][C:14]2[C:23]3[C:18](=[CH:19][C:20]([O:26][CH2:27][CH2:28][N:29](C)[C:30](OC(C)(C)C)=O)=[C:21]([O:24][CH3:25])[CH:22]=3)[N:17]=[CH:16][N:15]=2)=[C:11]([F:40])[CH:10]=1.C1(C)C=CC=CC=1>C(Cl)Cl>[OH2:2].[ClH:8].[Cl:8][C:9]1[CH:39]=[CH:38][C:12]([NH:13][C:14]2[C:23]3[C:18](=[CH:19][C:20]([O:26][CH2:27][CH2:28][NH:29][CH3:30])=[C:21]([O:24][CH3:25])[CH:22]=3)[N:17]=[CH:16][N:15]=2)=[C:11]([F:40])[CH:10]=1

参加物

5

反応物 3

HCID 1140TolueneHCID 6422Trifluoroacetic acidHCID 226250154-(4-chloro-2-fluoroanilino)-6-methoxy-7-(2-(N-methyl-N-t-butoxycarbonylamino)ethoxy)quinazoline

生成物 1

HCID 226249694-(4-Chloro-2-fluoroanilino)-6-methoxy-7-(2-(methylamino)ethoxy)quinazoline hydrochloride hydrate収率 79%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

TFA (4 ml) was added to a solution of 4-(4-chloro-2-fluoroanilino)-6-methoxy-7-(2-(N-methyl-N-t-butoxycarbonylamino)ethoxy)quinazoline (390 mg, 0.82 mmol) in methylene chloride (4 ml) and the mixture stirred for 2 hours at ambient temperature. Toluene was added and the volatiles were removed by evaporation. The residue was dissolved in methylene chloride and 3M ethereal hydrogen chloride (1 ml) was added. The resulting precipitate was collected by filtration, washed with ether and dried under vacuum to give 4-(4-chloro-2-fluoroanilino)-6-methoxy-7-(2-(methylamino)ethoxy)quinazoline hydrochloride hydrate (290 mg; 79%).

後処理

  1. customthe volatiles were removed by evaporation
  2. dissolutionThe residue was dissolved in methylene chloride
  3. addition3M ethereal hydrogen chloride (1 ml) was added
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with ether
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-848213cf70904cc39564ef68ffdf122d
出典データセット
uspto-grants-1999_10
特許番号
US05962458

反応ノート

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