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Methanol → HCID 135589776、化合物

HRID 384818
ノート
印刷プレビュー

反応式

HRID 384818 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:7]([C:8](OC)=[O:9])[C:6]([NH2:13])=[CH:5][C:4]=1[O:14][CH2:15][CH2:16][CH2:17][CH2:18][Cl:19].C([O-])([O-])OC.C([O-])(=O)C.[NH4+:29].[CH3:30]O>O>[CH3:1][O:2][C:3]1[CH:12]=[C:7]2[C:6](=[CH:5][C:4]=1[O:14][CH2:15][CH2:16][CH2:17][CH2:18][Cl:19])[N:13]=[CH:30][NH:29][C:8]2=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 517165Ammonium AcetateHCID 10286203HCID 10286203、化合物HCID 53629101Methylorthoformate

生成物 1

HCID 135589776HCID 135589776、化合物収率 96%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

In a 10 mL volume stainless pressure-resistant vessel equipped with a stirrer and a thermometer were placed 1.1 g (3.5 mmol) of methyl 5-methoxy-4-(4-chlorobutoxy)-anthranilate, 0.92 g (8.8 mmol) of methyl orthoformate, 0.67 g (8.8 mmol) of ammonium acetate, and 5 mL of methanol. The vessel was closed, and the reaction was carried out at 90-95° C. for 8 hours. After the reaction was complete, 50 mL of water was added to the reaction mixture. The aqueous reaction mixture was stirred at 25° C. for one hour, to precipitate a crystalline product. The crystalline product was collected by filtration and dried at 60° C. under reduced pressure, to give 0.94 g (isolated yield: 96%) of 6-methoxy-7-(4-chlorobutoxy)quinazolin-4-one as a gray crystalline product.

後処理

  1. customIn a 10 mL volume stainless pressure-resistant vessel equipped with a stirrer
  2. customThe vessel was closed
  3. customto precipitate a crystalline product
  4. filtrationThe crystalline product was collected by filtration
  5. customdried at 60° C. under reduced pressure

出典と根拠

ORDレコード
ord-d73df4b868e84452a857d9ecf90ea218
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367824B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート