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Benzene → 1-[(Dimethylamino)carbonyl]-1,6-dihydro-2-methoxy-4-methyl-6-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester

HRID 1722396
ノート
印刷プレビュー

反応式

HRID 1722396 の反応式
[CH3:1][O:2][C:3]1[NH:4][C:5]([CH3:24])=[C:6]([C:18]([O:20][CH:21]([CH3:23])[CH3:22])=[O:19])[CH:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=2)[N:8]=1.[CH2:25]([N:27]([CH2:30]C)[CH2:28]C)C.C(Cl)(Cl)=[O:33].C1C=CC=CC=1.CNC>ClCCl>[CH3:25][N:27]([CH3:30])[C:28]([N:8]1[CH:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=2)[C:6]([C:18]([O:20][CH:21]([CH3:22])[CH3:23])=[O:19])=[C:5]([CH3:24])[N:4]=[C:3]1[O:2][CH3:1])=[O:33]
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

7

反応物 5

HCID 241BenzeneHCID 674DimethylamineHCID 6371PhosgeneHCID 8471TriethylamineHCID 146271971,4-Dihydro-2-methoxy-6-methyl-4-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, 1-methyethyl ester

生成物 1

HCID 142570701-[(Dimethylamino)carbonyl]-1,6-dihydro-2-methoxy-4-methyl-6-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A solution of 1,4-dihydro-2-methoxy-6-methyl-4-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester (3.34 g, 10.0 mmol) and distilled triethylamine (6.3 ml, 45 mmol) in dichloromethane (10 ml) in an ice bath under argon was treated dropwise via syringe with 1.3M phosgene in benzene solution (9.2 ml, 12 mmol) over 3 to 5 minutes. After stirring at 0° C. for 1.5 hours, the reaction mixture was treated with 40% aqueous dimethylamine (3.3 ml, 15 mmol), capped with a septum, and stirred at room temperature for about 21/2 days. The reaction was then evaporated and partitioned between ethyl acetate and water. The organic phase was washed with saturated sodium chloride, dried (potassium carbonate), and evaporated to give the title compound (crude) as a brown oil (4.75 g).

後処理

  1. customcapped with a septum
  2. stirringstirred at room temperature for about 21/2 days
  3. customThe reaction was then evaporated
  4. custompartitioned between ethyl acetate and water
  5. washThe organic phase was washed with saturated sodium chloride
  6. dry with materialdried (potassium carbonate)
  7. customevaporated

出典と根拠

ORDレコード
ord-52535b42b91e49148ca9b4cec8165271
出典データセット
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04855301

反応ノート

読み込み中…

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