Water → 6-Fluoro-4-(2-(4-tert-butylphenyl)ethoxy)quinazoline

HRID 1516110

反応式

HRID 1516110 の反応式
[F-:1].[K+].C1N2CCOCCOCCN(CCOCCOCC2)CCOCCOC1.[N+]([C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][N:36]=[C:35]2[O:42][CH2:43][CH2:44][C:45]1[CH:50]=[CH:49][C:48]([C:51]([CH3:54])([CH3:53])[CH3:52])=[CH:47][CH:46]=1)([O-])=O.O>C1COCC1>[F:1][C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][N:36]=[C:35]2[O:42][CH2:43][CH2:44][C:45]1[CH:50]=[CH:49][C:48]([C:51]([CH3:54])([CH3:53])[CH3:52])=[CH:47][CH:46]=1

参加物

6

反応物 4

HCID 962WaterHCID 728012,2,2-CryptandHCID 522689Potassium FluorideHCID 596786596-Nitro-4-(2-(4-tert-butylphenyl)ethoxy)quinazoline

生成物 1

HCID 596786656-Fluoro-4-(2-(4-tert-butylphenyl)ethoxy)quinazoline

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a 25 ml round bottom flask is added potassium fluoride (82.6 mg, 1.42 mmol) and kryptofix 222 (0.53 g, 1.42 mmol). The above mixture is stirred in THF for 20 minutes after which 6-Nitro-4-(2-(4-tert-butylphenyl)ethoxy)quinazoline (0.1 g, 0.284 mmol) is added to it. The solution is refluxed for 30 minutes after which it is cooled and water is added to it. It is then extracted in dichloromethane, washed with water and dried. Purification by flash chromatography (silica gel; ethyl acetate/hexanes) gives the above compound.

後処理

  1. additionis added to it
  2. temperatureThe solution is refluxed for 30 minutes after which it
  3. temperatureis cooled
  4. extractionIt is then extracted in dichloromethane
  5. washwashed with water
  6. customdried
  7. customPurification by flash chromatography (silica gel; ethyl acetate/hexanes)
  8. customgives the above compound

出典と根拠

ORDレコード
ord-786f7e7def35486fa9fcd672115a4612
出典データセット
uspto-grants-2012_07
特許番号
US08226929B2

関連ノート

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