Sodium Carbonate → HCID 86655023、化合物

HRID 2066891ノート

反応式

HRID 2066891 の反応式
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

参加物

8

反応物 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

生成物 1

HCID 86655023HCID 86655023、化合物収率 135.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-8ba083ad998d4497a42915e08918ce7a
出典データセット
uspto-grants-2012_10
特許番号
US08293729B2

反応ノート

読み込み中…