Sodium → 4-Ethyl-5-methoxy-thiazol-2-ylamine
反応式
[CH3:1][O-:2].[Na+].[Na].Br[C:6]1[S:10][C:9]([NH2:11])=[N:8][C:7]=1[CH2:12][CH3:13]>CO>[CH2:12]([C:7]1[N:8]=[C:9]([NH2:11])[S:10][C:6]=1[O:2][CH3:1])[CH3:13]参加物
5
反応条件
- 温度
- 0 °C
実験手順
Sodium methoxide was freshly prepared by dissolving 0.186 g (8.1 mmol) of sodium metal in 12 mL of abs. MeOH. After cooling to 0° C., 5-bromo-4-ethyl-thiazol-2-ylamine (0.519 g, 2.51 mmol) was added and the cooling bath removed. After 45 min, TLC indicated the absence of starting material. The reaction mixture was poured onto crashed ice, twofold extracted with ethyl acetate, washed with brine, dried over sodium sulfate, and evaporated to dryness. Thereby, 0.298 g of the title compound was obtained as brown, rather unstable oil, sufficiently pure to be used for the next step; it should be stored at −28° C.
後処理
- customthe cooling bath removed
- additionThe reaction mixture was poured
- extractiontwofold extracted with ethyl acetate
- washwashed with brine
- dry with materialdried over sodium sulfate
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-0676b8d7e9e84256a98815705d66bc59
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07973051B2
反応ノート
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