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

HRID 384763ノート

反応式

HRID 384763 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-79064fdb8a874f8f926860e49a31b8e8
出典データセット
uspto-grants-2013_02
特許番号
US08367824B2

反応ノート

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