Ammonium Acetate → 6,7-Bis(2-methoxyethoxy)quinazolin-4(3H)-one

HRID 384763노트

반응식

HRID 384763 반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([NH2:20])[C:9](=[CH:13][C:14]=1[O:15][CH2:16][CH2:17][O:18][CH3:19])[C:10](O)=[O:11].[CH:21]([O-])([O-])OC.C([O-])(=O)C.[NH4+:30]>CO>[CH3:19][O:18][CH2:17][CH2:16][O:15][C:14]1[CH:13]=[C:9]2[C:8](=[CH:7][C:6]=1[O:5][CH2:4][CH2:3][O:2][CH3:1])[N:20]=[CH:21][NH:30][C:10]2=[O:11]

참가 물질

5

반응물 3

HCID 517165Ammonium AcetateHCID 230330092-Amino-4,5-bis(2-methoxyethoxy)benzoic acidHCID 53629101Methylorthoformate

생성물 1

HCID 1354093056,7-Bis(2-methoxyethoxy)quinazolin-4(3H)-one수율 103.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a 10-mL volume stainless steel pressure-resistant vessel were placed 1.00 g (2.8 mmol) of 4,5-bis(2-methoxyethoxy)anthranilic acid, 0.93 g (8.8 mmol) of methyl orthoformate, 0.67 g (8.8 mmol) of ammonium acetate, and 5.0 mL of methanol. The reaction was carried out at 95° C. for 8 hours. After the reaction was complete, the reaction mixture was cooled to room temperature and concentrated under reduced pressure. Then, the concentrate was recrystallized from 20 mL of methanol. The crystalline product was collected by filtration and dried under reduced pressure to give 0.85 g (isolated yield: 83%) of 6,7-bis(2-methoxyethoxy)quinazolin-4-one as a white crystalline product.

후처리

  1. customIn a 10-mL volume stainless steel pressure-resistant vessel were placed
  2. concentrationconcentrated under reduced pressure
  3. customThen, the concentrate was recrystallized from 20 mL of methanol
  4. filtrationThe crystalline product was collected by filtration
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-79064fdb8a874f8f926860e49a31b8e8
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367824B2

반응 노트

불러오는 중…