Urea → HCID 12023321, 화합물

HRID 2236567노트

반응식

HRID 2236567 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

HCID 12023321HCID 12023321, 화합물수율 34%

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-4a9437c76226460d995d0aaa045cb8c5
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

반응 노트

불러오는 중…