Potassium Carbonate → 4-(2-Chloro-4-formyl-phenoxy)-benzamide

HRID 130951

反応式

HRID 130951 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1F)[CH:5]=[O:6].[OH:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([NH2:18])=[O:17])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+].CC(N(C)C)=O>O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[O:6])[CH:7]=[CH:8][C:9]=1[O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([NH2:18])=[O:17])=[CH:14][CH:13]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 31374DimethylacetamideHCID 650524-HydroxybenzamideHCID 5938663-Chloro-4-fluorobenzaldehyde

生成物 1

HCID 597302874-(2-Chloro-4-formyl-phenoxy)-benzamide収率 94%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Mix 3-chloro-4-fluorobenzaldehyde (3.28 g, 20.7 mmol), 4-hydroxybenzamide (3.12 g, 22.7 mmol), potassium carbonate (4.29 g, 31.0 mmol) and dimethylacetamide (80 mL) in a flask. Heat the reaction to 100° C. for 3 hours. Let cool to ambient (room) temperature and pour into water (200 mL). After trituration, filter the solid formed and dry on a vacuum pump to obtain the product (5.35 g, 94%). 1H NMR (DMSO-d6) 9.94 (s, 1H), 8.13 (d, J=1.7 Hz, 1H), 7.98 (bs, 1H), 7.94 (d, J=8.5 Hz, 2H), 7.88 (dd, J=1.7 Hz, 8.5 Hz, 1H), 7.36 (bs, 1H), 7.21 (d, J=8.5 Hz, 1H), 7.14 (d, J=8.5 Hz, 2H).

後処理

  1. temperatureHeat
  2. customthe reaction to 100° C. for 3 hours
  3. temperatureLet cool to ambient (room) temperature
  4. filtrationAfter trituration, filter the solid
  5. customformed
  6. customdry on a vacuum pump

出典と根拠

ORDレコード
ord-9a8b9b56d6534aa88af249f992085103
出典データセット
uspto-grants-2008_06
特許番号
US07381719B2

関連ノート

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