Urea → HCID 178487639, 화합물

HRID 2079617

반응식

HRID 2079617 반응식
[CH:1]([C:3]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:4]=1[NH2:5])=O.[NH2:12][C:13](N)=[O:14]>O>[OH:14][C:13]1[N:12]=[CH:1][C:3]2[C:4](=[CH:6][C:7]([O:10][CH3:11])=[CH:8][CH:9]=2)[N:5]=1

참가 물질

4

반응물 2

HCID 1176UreaHCID 3235032-Amino-4-methoxybenzaldehyde

생성물 1

HCID 178487639HCID 178487639, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
175 °C

실험 절차

2-Formyl-5-methoxyaniline (11.93 g, 79.5 mmol, 1.0 eq) and urea (38.0 g, 0.636 mol, 8.0 eq) were mixed, ground into a fine powder and placed into a 1 L 2-neck flask equipped with a mechanical stirrer and an air condenser. The flask was placed into a preheated (160° C.) oil bath. The reaction mixture melted and was stirred at 170-180° C. for 1 hour until it solidified forming yellowish-brown solid. The reaction mixture was cooled to RT, crushed, mixed with 70 mL of H2O and stirred for ˜1 hour at RT. The solid was filtered, washed with 150 mL of H2O and 20 mL of ice cold Et2O. The yellow solid thus obtained was dried over P4O10 under high vacuum for several hours and the crude material (12.57 g) was used for the next step without purification.

후처리

  1. customequipped with a mechanical stirrer and an air condenser
  2. customwas placed into a preheated (160° C.) oil bath
  3. customsolidified forming yellowish-brown solid
  4. temperatureThe reaction mixture was cooled to RT
  5. customcrushed
  6. stirringstirred for ˜1 hour at RT
  7. filtrationThe solid was filtered
  8. washwashed with 150 mL of H2O and 20 mL of ice cold Et2O
  9. customThe yellow solid thus obtained
  10. dry with materialwas dried over P4O10 under high vacuum for several hours
  11. customthe crude material (12.57 g) was used for the next step without purification

출처 및 근거

ORD 기록
ord-e53372179d344de9a4355461e84c14f5
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932262B2

연결된 노트

불러오는 중…