Sodium Hydroxide → 2-Amino-4-(3,5-diacetylphenyl)imino-1,4-dihydro-1,6-dimethylpyrimidine

HRID 480410

反応式

HRID 480410 の反応式
[I-].[NH2:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2[CH:15]=[C:14]([C:16](=[O:18])[CH3:17])[CH:13]=[C:12]([C:19](=[O:21])[CH3:20])[CH:11]=2)[CH:6]=[C:5]([CH3:22])[N+:4]=1[CH3:23].CO.O.[OH-].[Na+]>O>[NH2:2][C:3]1[N:4]([CH3:23])[C:5]([CH3:22])=[CH:6][C:7](=[N:9][C:10]2[CH:11]=[C:12]([C:19](=[O:21])[CH3:20])[CH:13]=[C:14]([C:16](=[O:18])[CH3:17])[CH:15]=2)[N:8]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 98453522-Amino-4-(3,5-diacetylphenyl)amino-1,6-dimethylpyrimidinium iodideHCID 22242641Methanol--water (1/1)

生成物 1

HCID 730892-Amino-4-(3,5-diacetylphenyl)imino-1,4-dihydro-1,6-dimethylpyrimidine収率 99.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

A suspension of 21 g (49.3 mmole) of 2-amino-4-(3,5-diacetylphenyl)amino-1,6-dimethylpyrimidinium iodide (compound No. 2, synthesized as described in section 6.1) in 1:1 methanol/water (750 mL) at 60° C. was treated with excess 2N NaOH with cooling to maintain about 60° C. An additional 200 mL of water was added and the mixture was cooled in ice and filtered to give 14.69 g 2-amino-4-(3,5-diacetylphenyl) imino-1,4-dihydro-1,6-dimethylpyrimidine as yellow crystals, mp 219-220°.

後処理

  1. temperaturewith cooling
  2. temperaturethe mixture was cooled in ice
  3. filtrationfiltered

出典と根拠

ORDレコード
ord-46f358ec0fb94b93b1b1f6073b8d498a
出典データセット
uspto-grants-2003_11
特許番号
US06649797B2

関連ノート

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