Dimethylformamide dimethyl acetal → HCID 68706092、化合物

HRID 2232963ノート

反応式

HRID 2232963 の反応式
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>>[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([N:6]=[CH:14][N:15]([CH3:17])[CH3:16])=[O:5]

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 27359562,3-Dichlorobenzamide

生成物 1

HCID 68706092HCID 68706092、化合物

実験手順

2,3-Dichlorobenzamide (4.96 g, 26.1 mmol) and dimethylformamide dimethylacetal (10 mL) were heated at reflux for 1.5 hours, allowed to cool to room temperature, concentrated under reduced pressure, and the residue was partitioned between diethyl ether and water. The organic phase was washed with water (2×), saturated sodium chloride, dried with sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography eluting with ethyl acetate to provide the title compound. MS (DCI/NH3) m/z 245 (M+H)+.

後処理

  1. temperatureat reflux for 1.5 hours
  2. concentrationconcentrated under reduced pressure
  3. customthe residue was partitioned between diethyl ether and water
  4. washThe organic phase was washed with water (2×), saturated sodium chloride
  5. dry with materialdried with sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe residue was purified by flash chromatography
  9. washeluting with ethyl acetate

出典と根拠

ORDレコード
ord-5d7a81d5dcaa4807b9829a58aeaebb76
出典データセット
uspto-grants-2010_05
特許番号
US07709469B2

反応ノート

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