Urea → HCID 12023321、化合物

HRID 2236567ノート

反応式

HRID 2236567 の反応式
[C:1]([CH2:4][C:5]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:6]=1[C:7](O)=[O:8])(O)=[O:2].[NH2:15]C(N)=O>>[Cl:14][C:12]1[CH:13]=[C:5]2[C:6](=[CH:10][CH:11]=1)[C:7](=[O:8])[NH:15][C:1](=[O:2])[CH2:4]2

参加物

3

反応物 2

HCID 1176UreaHCID 3340352-(Carboxymethyl)-4-chlorobenzoic acid

生成物 1

HCID 12023321HCID 12023321、化合物収率 34%

実験手順

An amount of 2-(carboxymethyl)-4-chlorobenzoic acid (8.4 g, 39.14 mmol) and 2.82 g (47 mmol) of urea is vigorously stirred at 160° C. Solids were melted, boiled and hardened after 15 min. Continue to heat and blow nitrogen through to remove water generated from reaction until total dryness. After cooling, the solid is ground to fine powder. After successively washing with saturated NaHCO3 solution, water, methanol, ether and hexane, the powder is dried in oven (60° C.) overnight to give 2.6 g (34.0% yield) of light yellow solid: MS (ESI) m/z 194.0 (M−H)−1 Analysis for C9H6ClNO2, Calcd: C, 55.26; H, 3.09; N, 7.16. Found: C, 54.86; H, 2.96; N, 7.12

後処理

  1. temperatureto heat
  2. customto remove water
  3. customgenerated from reaction until total dryness
  4. temperatureAfter cooling
  5. washAfter successively washing with saturated NaHCO3 solution, water, methanol, ether and hexane
  6. customthe powder is dried in oven (60° C.) overnight
  7. customto give 2.6 g (34.0% yield) of light yellow solid

出典と根拠

ORDレコード
ord-4a9437c76226460d995d0aaa045cb8c5
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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