Benzyl Bromide → HCID 21891956、化合物

HRID 2304557ノート

反応式

HRID 2304557 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:17]([CH:18]=[O:19])=[CH:16][C:15]2[C:10](=[CH:11][C:12]([F:21])=[C:13]([OH:20])[CH:14]=2)[N:9]=1.[CH2:22](Br)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>CN(C)C=O>[CH2:22]([O:20][C:13]1[CH:14]=[C:15]2[C:10](=[CH:11][C:12]=1[F:21])[N:9]=[C:8]([Cl:7])[C:17]([CH:18]=[O:19])=[CH:16]2)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 21892040HCID 21892040、化合物

生成物 1

HCID 21891956HCID 21891956、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

Potassium carbonate (9.2 g, 66 mmol) is added to a solution of 2-chloro-7-fluoro-6-hydoxy-3-quinolinecarbaldehyde (obtained according to 1.c, 13 g, 58 mmol) in anhydrous N,N-dimethylformamide (120 ml) and the mixture, placed under an argon atmosphere, is cooled down to 0° C. Benzyl bromide (7.9 ml, 66 mmol) is added dropwise and the reaction medium is maintained under agitation at ambient temperature for 16 hours. The reaction medium is then poured into ice cold water (200 ml) and the resulting yellow solid is filtered, then taken up in ethanol (200 ml) and concentrated under reduced pressure. The residue is taken up in ethyl ether (200 ml) and the resulting yellow solid is filtered then dried under reduced pressure in order to produce 15 g (82%) of a yellow solid, m.p. 228° C.

後処理

  1. temperaturethe reaction medium is maintained under agitation at ambient temperature for 16 hours
  2. filtrationthe resulting yellow solid is filtered
  3. concentrationconcentrated under reduced pressure
  4. filtrationthe resulting yellow solid is filtered
  5. customthen dried under reduced pressure in order

出典と根拠

ORDレコード
ord-e1c5daaabefb431ea5f0d8310e37535d
出典データセット
uspto-grants-2002_08
特許番号
US06436951B1

反応ノート

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