Sodium Carbonate → HCID 86655023, 화합물

HRID 2066891노트

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HRID 2066891 반응식
C(=O)(O)[O-].[Na+].[NH:6]1[CH2:11][CH2:10][CH:9]([O:12][N:13]=[C:14]2[CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][C:23]([S:26]([CH3:29])(=[O:28])=[O:27])=[CH:22][C:21]=3[F:30])[CH2:16][CH2:15]2)[CH2:8][CH2:7]1.[N:31]#[C:32]Br.C(=O)([O-])[O-].[Na+].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl.O>[F:30][C:21]1[CH:22]=[C:23]([S:26]([CH3:29])(=[O:27])=[O:28])[CH:24]=[CH:25][C:20]=1[N:17]1[CH2:18][CH2:19][C:14](=[N:13][O:12][CH:9]2[CH2:10][CH2:11][N:6]([C:32]#[N:31])[CH2:7][CH2:8]2)[CH2:15][CH2:16]1

참가 물질

8

반응물 5

HCID 10340Sodium CarbonateHCID 10476Cyanogen BromideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 516892Sodium BicarbonateHCID 866550221-(2-Fluoro-4-methanesulfonyl-phenyl)-piperidin-4-one O-piperidin-4-yl-oxime

생성물 1

HCID 86655023HCID 86655023, 화합물수율 135.6%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To sodium bicarbonate (34 mg, 0.4 mmol), was added water (17 μL) and 63a (74 mg, 0.2 mmol) in 1 mL of DCM. The mixture was cooled to 0° C. and cyanogen bromide (25 mg, 0.24 mmol) was added. The mixture was stirred at room temperature overnight. Sodium carbonate was added as well as magnesium sulfate and the solids were filtered and rinsed with DCM. The filtrate was concentrated to give 107 mg of 68b.

후처리

  1. filtrationthe solids were filtered
  2. washrinsed with DCM
  3. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-8ba083ad998d4497a42915e08918ce7a
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293729B2

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