Iodoethane → 5-Chloro-2-ethoxybenzamide

HRID 437423

反応式

HRID 437423 の反応式
[Cl:1][C:2]1[CH:10]=[C:6]([C:7]([NH2:9])=[O:8])[C:5]([OH:11])=[CH:4][CH:3]=1.I[CH2:13][CH3:14].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:13][CH3:14])=[C:6]([CH:10]=1)[C:7]([NH2:9])=[O:8]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 3480945-Chloro-2-hydroxybenzamide

生成物 1

HCID 203602935-Chloro-2-ethoxybenzamide収率 36.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 5-chlorosalicylamide (16.0 g., 0.093 mole), iodoethane (31.8 g., 0.204 mole), and potassium carbonate (13.1 g., 0.095 mole) in ethanol (225 ml.) was heated under reflux for 20 hours. The hot mixture was filtered. The filtrate was reduced to dryness. The residue was triturated with water. The mixture was filtered and the collected solid recrystallized from acetonitrile to give 5-chloro-2-ethoxybenzamide (6.8 g., 36.6%) m.p. 136°-139°.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 20 hours
  3. filtrationThe hot mixture was filtered
  4. customThe residue was triturated with water
  5. filtrationThe mixture was filtered
  6. customthe collected solid recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-a41ab30757f346f09213a2bfca4b3c19
出典データセット
uspto-grants-1977_06
特許番号
US04031093

関連ノート

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