반응식
C1CNCCN1.FC1(F)Oc2ccc(Br)cc2O1>C1COCCO1.CC(C)(C)P(C(C)(C)C)C(C)(C)C.CC(C)(C)P(C(C)(C)C)C(C)(C)C.CC(C)(C)P(C(C)(C)C)C(C)(C)C.CC(C)(C)[O-].[K+].[Pd]>FC1(F)Oc2ccc(N3CCNCC3)cc2O1참가 물질
7
반응물 2
생성물 1
시약·촉매·용매 4
반응 조건
- 온도
- 90 °C
실험 절차
13-May-09 10:32:07 +0100 5-bromo-2,2-difluorobenzo[d][1,3]dioxole (0.500 g, 2.11 mmol), piperazine (0.182 g, 2.11 mmol) and BIS(TRI-T-BUTYLPHOSPHINE)PALLADIUM(0) (0.054 g, 0.11 mmol) and potassium 2-methylpropan-2-olate (0.349 g, 2.95 mmol) were suspended in dioxane (10vol) (10 mL) and heated to 90°C for 1 hour. LC-MS shows no starting material 52% product and 41% dimer. The reaction mixture was combined with EN02263-54 filtered and the crude product was purified by flash silica chromatography, elution gradient 0 to 10% MeOH in DCM. Pure fractions were evaporated to dryness to afford 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)piperazine (0.259 g, 50.7 %) as a yellow oil.
출처 및 근거
- ORD 기록
- ord-a6f7db18dd5949e09df857ba4df0f8b1
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
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