Sodium → 5-Methoxy-4-methyl-thiazol-2-ylamine
반응식
[CH3:1][O-:2].[Na+].[Na].Br[C:6]1[S:10][C:9]([NH2:11])=[N:8][C:7]=1[CH3:12]>CO>[CH3:1][O:2][C:6]1[S:10][C:9]([NH2:11])=[N:8][C:7]=1[CH3:12]참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
Sodium methoxide was freshly prepared by dissolving 0.408 g (17.7 mmol) of sodium metal in 25 mL of abs. MeOH. After cooling to 0° C., 5-bromo-4-methyl-thiazol-2-ylamine (1.00 g, 5.18 mmol) was added and the cooling bath removed. After 15 Min., TLC indicated the absence of starting material. The reaction mixture was poured onto crashed ice/NH4Cl, twofold extracted with ethyl acetate, washed with water, dried over sodium sulfate, and evaporated to dryness. Flash chromatography (SiO2, hexane/ethyl acetate=1/1), yielded 0.441 g of the title compound as brown oil; it should be stored at −28° C.
후처리
- customthe cooling bath removed
- additionThe reaction mixture was poured
- extractiontwofold extracted with ethyl acetate
- washwashed with water
- dry with materialdried over sodium sulfate
- customevaporated to dryness
출처 및 근거
- ORD 기록
- ord-3c3ad3175a7f43a687cc2e1d67a87728
- 출처 데이터셋
- uspto-grants-2011_07
- 특허 번호
- US07973051B2
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