Water → HCID 18331085、化合物

HRID 2270053ノート

反応式

HRID 2270053 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12](=[O:15])[CH2:13]Br)=[CH:8][CH:7]=1)=[O:5])[CH3:2].[N-:16]=[N+:17]=[N-:18].[Na+].O>CN(C)C=O>[N:16]([CH2:13][C:12]([C:9]1[CH:10]=[CH:11][C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])=[CH:7][CH:8]=1)=[O:15])=[N+:17]=[N-:18]

参加物

5

反応物 3

HCID 962WaterHCID 33557Sodium AzideHCID 11966043Ethyl 4-(2-bromoacetyl)benzoate

生成物 1

HCID 18331085HCID 18331085、化合物収率 84.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4′-ethoxycarbonyl-2-bromoacetophenone (2.0 g) in N,N-dimethylformamide (8 ml) was added sodium azide (480 mg) at 0° C., and stirred for 2 hours at room temperature. The reaction mixture was poured into water (100 ml), extracted with diethyl ether (200 ml×2), washed with brine, and dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure. The product was purified by silica gel column chromatography (ethyl acetate:hexane=1:5) to give 2-azido-4′-ethoxycarbonylacetophenone (1.46 g).

後処理

  1. extractionextracted with diethyl ether (200 ml×2)
  2. washwashed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationMagnesium sulfate was filtered off
  5. customthe filtrate was evaporated under reduced pressure
  6. customThe product was purified by silica gel column chromatography (ethyl acetate:hexane=1:5)

出典と根拠

ORDレコード
ord-0826fe863e664bf7a30270f5d657859b
出典データセット
uspto-grants-2001_12
特許番号
US06331521B1

反応ノート

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