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Water → 4-Chloro-5-ethyl-2-thiophenecarboxaldehyde

HRID 221055
ノート
印刷プレビュー

反応式

HRID 221055 の反応式
[CH2:1]([C:3]1[S:7][C:6]([CH:8]=[O:9])=[CH:5][CH:4]=1)[CH3:2].[Cl:10]N1C(=O)CCC1=O.O>CN(C)C=O>[Cl:10][C:4]1[CH:5]=[C:6]([CH:8]=[O:9])[S:7][C:3]=1[CH2:1][CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 31398Chlorosuccinimide2 回HCID 1698305-Ethyl-2-thiophenecarboxaldehyde

生成物 1

HCID 838743164-Chloro-5-ethyl-2-thiophenecarboxaldehyde収率 41.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5-ethyl-2-thiophenecarboxaldehyde (6.0 g) in N,N-dimethylformamide (60 ml) was added N-chlorosuccinimide (8.57 g), and the mixture was stirred at room temperature for 2 hours, and subsequently stirred under heating at 60° C. for 2 hours. N-chlorosuccinimide (4.00 g) was further added thereto, and the mixture was further stirred under heating at 60° C. for 2 hours. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate, washed with brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=33:1) to give 4-chloro-5-ethyl-2-thiophenecarboxaldehyde (3.1 g) as colorless oil. (2) The above 4-chloro-5-ethyl-2-thiophenecarboxaldehyde was treated in a manner similar to Reference Example 1 to give 3-bromo-1-(4-chloro-5-ethyl-2-thienylmethyl)benzene as yellow oil. APCI-Mass m/Z 347/349 (M+H+MeOH).

後処理

  1. stirringsubsequently stirred
  2. temperatureunder heating at 60° C. for 2 hours
  3. stirringthe mixture was further stirred
  4. temperatureunder heating at 60° C. for 2 hours
  5. extractionthe mixture was extracted with ethyl acetate
  6. washwashed with brine
  7. dry with materialdried over sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=33:1)

出典と根拠

ORDレコード
ord-013185b1457e450d8cb505bf2cd60f3f
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202984B2

反応ノート

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