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Ethyl 2-(4,6-dimethyl-5-nitropyrimidine-2-yloxy)acetate → Ethyl 2-(5-amino-4,6-dimethylpyrimidine-2-yloxy)acetate

HRID 2280889
ノート
印刷プレビュー

反応式

HRID 2280889 の反応式
[CH3:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([CH3:11])[N:5]=[C:4]([O:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:3]=1.[H][H]>C(O)C.[Pd]>[NH2:8][C:7]1[C:2]([CH3:1])=[N:3][C:4]([O:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[N:5][C:6]=1[CH3:11]
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

5

反応物 2

HCID 59336196Ethyl 2-(4,6-dimethyl-5-nitropyrimidine-2-yloxy)acetateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 59336106Ethyl 2-(5-amino-4,6-dimethylpyrimidine-2-yloxy)acetate収率 99.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

反応条件

温度
25 °C

実験手順

Compound 6 (75.98 g) and 5% Pd—C (7.598 g, N. E. CHEMCAT, STD Type) were suspended in ethanol (760 mL). Evacuation and replacement with hydrogen were repeated three times. Subsequently, the suspension was vigorously stirred at room temperature (20 to 30° C.) for 4.5 hours under hydrogen atmosphere. After the reaction was completed, the mixture was subjected to high precision pressure filtration (0.2 μm, PTFE) and the filtered product was washed with ethanol (474 mL). The filtrate was evaporated under reduced pressure to give 66.99 g (99.9% yield) of the desired product as a pale yellow solid.

後処理

  1. filtrationthe mixture was subjected to high precision pressure filtration (0.2 μm, PTFE)
  2. washthe filtered product was washed with ethanol (474 mL)
  3. customThe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-360173c0d7e94654a80bd4f0de06a275
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09139559B2

反応ノート

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