Methanol → 6-Iodoquinazolin-4-one

HRID 384754

反応式

HRID 384754 の反応式
[I:1][C:2]1[CH:10]=[C:6]([C:7](O)=[O:8])[C:5]([NH2:11])=[CH:4][CH:3]=1.C([O-])([O-])OC.C([O-])(=O)C.[NH4+:21].[CH3:22]O>O>[I:1][C:2]1[CH:10]=[C:6]2[C:5](=[CH:4][CH:3]=1)[N:11]=[CH:22][NH:21][C:7]2=[O:8]

参加物

6

反応物 4

HCID 887MethanolHCID 72911Benzoic acid, 2-amino-5-iodo-HCID 517165Ammonium AcetateHCID 53629101Methylorthoformate

生成物 1

HCID 1354016666-Iodoquinazolin-4-one収率 93%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In a 10-mL volume stainless steel pressure-resistant vessel were placed 1.0 g (3.8 mmol) of 5-iodoanthranilic acid, 0.81 g (7.6 mmol) of methyl orthoformate, 0.59 g (7.6 mmol) of ammonium acetate, and 4.0 mL of methanol. The reaction was carried out at 120° C. for 3 hours. After the reaction was complete, the reaction mixture was cooled to room temperature, and 40 mL of water was added to the reaction mixture. The resulting aqueous mixture was stirred for 15 minutes and filtered to give 0.97 g (isolated yield: 93%) of 6-iodoquinazolin-4-one as a pale gray crystalline product.

後処理

  1. customIn a 10-mL volume stainless steel pressure-resistant vessel were placed
  2. filtrationfiltered

出典と根拠

ORDレコード
ord-e0cee7944b3d4854b339820c84655ba9
出典データセット
uspto-grants-2013_02
特許番号
US08367824B2

関連ノート

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