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2,2'-Bipyridine → 4-(benzyloxy)-6-chloro-3-cyclopropyl-3H-imidazo[4,5-c]pyridine

HRID 2209007
ノート
印刷プレビュー

反応式

HRID 2209007 の反応式
[CH2:1]([O:8][C:9]1[C:14]2[NH:15][CH:16]=[N:17][C:13]=2[CH:12]=[C:11]([Cl:18])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:19]1(B(O)O)[CH2:21][CH2:20]1.C([O-])([O-])=O.[Na+].[Na+].B(O)O.N1C=CC=CC=1C1C=CC=CN=1>ClCCCl.CCOC(C)=O.CC([O-])=O.CC([O-])=O.[Cu+2]>[CH2:1]([O:8][C:9]1[C:14]2[N:15]([CH:19]3[CH2:21][CH2:20]3)[CH:16]=[N:17][C:13]=2[CH:12]=[C:11]([Cl:18])[N:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 14742,2'-BipyridineHCID 10340Sodium Carbonate4 回HCID 61668Boronic Acid3 回HCID 2760897Cyclopropylboronic acidHCID 178477827HCID 178477827、化合物

生成物 1

HCID 1178430004-(benzyloxy)-6-chloro-3-cyclopropyl-3H-imidazo[4,5-c]pyridine

試薬・触媒・溶媒 3

HCID 8895Cupric acetate触媒HCID 111,2-Dichloroethane溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

In a separate flask 4-(benzyloxy)-6-chloro-3H-imidazo[4,5-c]pyridine 2.24 (502 mg, 1.93 mmol), cyclopropane boronic acid (334 mg, 3.89 mmol) and Na2CO3 (415 mg, 3.9 mmol) were taken up in 1,2-DCE (13 mL). The aforementioned catalyst mixture was then added to this mixture, washing with 4×1 mL 1,2-DCE. The resulting mixture was heated to 70° C. and was stirred open to the air. After 7 h, additional Na2CO3 (215 mg, 2.03 mmol) and boronic acid (170 mg, 2.0 mmol) were added along with a heated suspension of Cu(OAc)2 (182 mg, 1.0 mmol) and 2,2′-bipyridine (155 mg, 0.99 mmol) in 1,2-DCE (3 mL). After an additional 1.5 h, additional boronic acid (340 mg, 4.0 mmol) and Na2CO3 (415 mg, 3.9 mmol) were added and the reaction was capped and stirred overnight. After an additional 14.5 h, additional boronic acid (150 mg, 1.7 mmol) and Na2CO3 (215 mg, 2.03 mmol) were added and the mixture was stirred open to air. After an additional 1.5 h, the reaction mixture was cooled to r.t., was diluted with EtOAc (75 mL), and was filtered through Celite. The filtrate was washed with half-saturated aqueous NH4Cl (75 mL), water (50 mL), and brine (50 mL). The organic phase was dried over Na2SO4, filtered, and concentrated. Purification by silica gel chromatography (0% to 5% THF in DCM) provided 4-(benzyloxy)-6-chloro-3-cyclopropyl-3H-imidazo[4,5-c]pyridine 2.35.

後処理

  1. additionThe aforementioned catalyst mixture was then added to this mixture
  2. washwashing with 4×1 mL 1,2-DCE
  3. waitAfter an additional 1.5 h
  4. customthe reaction was capped
  5. stirringstirred overnight
  6. waitAfter an additional 14.5 h
  7. stirringthe mixture was stirred open to air
  8. waitAfter an additional 1.5 h
  9. temperaturethe reaction mixture was cooled to r.t.
  10. filtrationwas filtered through Celite
  11. washThe filtrate was washed with half-saturated aqueous NH4Cl (75 mL), water (50 mL), and brine (50 mL)
  12. dry with materialThe organic phase was dried over Na2SO4
  13. filtrationfiltered
  14. concentrationconcentrated
  15. customPurification by silica gel chromatography (0% to 5% THF in DCM)

出典と根拠

ORDレコード
ord-c393bf07b92443a58e7fb724b84ef202
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09376441B2

反応ノート

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