Triethylamine → 3-(2-Fluoro-4-iodophenyl)-4-fluoro-8-methyl-1H-imidazo[4,5-g]quinazolin-2(3H)-one

HRID 558249ノート

反応式

HRID 558249 の反応式
[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[C:19]([F:20])=[C:18]2[C:13]([C:14]([CH3:21])=[N:15][CH:16]=[N:17]2)=[CH:12][C:11]=1C(O)=O.C([N:27]([CH2:30]C)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:39])C=CC=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:10]2[C:11](=[CH:12][C:13]3[C:14]([CH3:21])=[N:15][CH:16]=[N:17][C:18]=3[C:19]=2[F:20])[NH:27][C:30]1=[O:39]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 595194867-(2-Fluoro-4-iodophenylamino)-8-fluoro-4-methylquinazoline-6-carboxylic acid

生成物 1

HCID 595194923-(2-Fluoro-4-iodophenyl)-4-fluoro-8-methyl-1H-imidazo[4,5-g]quinazolin-2(3H)-one収率 75%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a suspension of 7-(2-fluoro-4-iodophenylamino)-8-fluoro-4-methylquinazoline-6-carboxylic acid (190 mg, 0.47 mmol) in toluene (10 ml) was added triethylamine (0.19 ml, 1.41 mmol) and diphenylphosphoryl azide (0.20 ml, 0.94 mmol). The reaction was heated at reflux for 4 h. The mixture was cooled to room temperature and concentrated to dryness. Silica gel chromatography (EtOAc:Hexane=75:25) yields 143 mg (75%) of the title compound as a tan solid.

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 4 h
  3. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-2338a7a50b234ca7bb76913c34192fa5
出典データセット
uspto-grants-2011_11
特許番号
US08063049B2

反応ノート

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