Potassium Carbonate → HCID 58020135、化合物

HRID 1632086ノート

反応式

HRID 1632086 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([CH2:8][CH2:9]Br)[CH:5]=[CH:4][C:3]=1[O:11][CH3:12].[OH:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1.C([O-])([O-])=O.[K+].[K+]>COCCOC>[Br:1][C:2]1[CH:7]=[C:6]([CH2:8][CH2:9][N:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]2=[O:13])[CH:5]=[CH:4][C:3]=1[O:11][CH3:12]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 58020164860584-79-8HCID 178516071HCID 178516071、化合物

生成物 1

HCID 58020135HCID 58020135、化合物収率 40%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

Into a 100 mL round bottom flask was added 2-bromo-4-(2-bromo-ethyl)-1-methoxy-benzene (I-165, 1.82 g, crude), 2-hydroxypyridine (258 mg, 2.72 mmol), K2CO3 (625 mg, 4.53 mmol), and DME (20 mL). After stirring for 18 hours at 80° C. the suspension was filtered and the filtrate was concentrated. The residue was purified by flash column chromatography eluting with 25-50% acetone/hexanes to afford 221 mg of I-166 as a brown oil in 40% yield (2 steps).

後処理

  1. filtrationwas filtered
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by flash column chromatography
  4. washeluting with 25-50% acetone/hexanes
  5. customto afford 221 mg of I-166 as a brown oil in 40% yield (2 steps)

出典と根拠

ORDレコード
ord-fbce92b0c78d42c8b73f6cbf18468173
出典データセット
uspto-grants-2014_07
特許番号
US08791267B2

反応ノート

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