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Dimethyl Sulfoxide → 4-[2-(Cyclohexylmethyl-amino)-benzooxazol-6-yloxy]-pyridine-2-carbonitrile

HRID 2370505
ノート
印刷プレビュー

反応式

HRID 2370505 の反応式
CS(C)=O.C(Cl)(=O)C(Cl)=O.[CH:11]1([CH2:17][NH:18][C:19]2[O:20][C:21]3[CH:27]=[C:26]([O:28][C:29]4[CH:34]=[CH:33][N:32]=[C:31]([C:35]([NH2:37])=O)[CH:30]=4)[CH:25]=[CH:24][C:22]=3[N:23]=2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.C(N(CC)CC)C>C(Cl)Cl>[CH:11]1([CH2:17][NH:18][C:19]2[O:20][C:21]3[CH:27]=[C:26]([O:28][C:29]4[CH:34]=[CH:33][N:32]=[C:31]([C:35]#[N:37])[CH:30]=4)[CH:25]=[CH:24][C:22]=3[N:23]=2)[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 57725827HCID 57725827、化合物

生成物 1

HCID 577257694-[2-(Cyclohexylmethyl-amino)-benzooxazol-6-yloxy]-pyridine-2-carbonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of the methylsulfoxide (32 mg, 0.41 mmol, 6.0 eq) in 1 mL of methylene chloride was added oxalyl chloride (2M, 0.135 mL, 0.27 mmol, 4.0 eq) at −78° C. After 15 minutes, the 4-(2-(cyclohexylmethylamino)benzo[d]oxazol-6-yloxy)pyridine-2-carboxamide (25 mg, 0.068 mmol, 1.0 eq) in 2 mL of methylene chloride was added to the reaction mixture. After being stirred at that temperature for 20 minutes, triethyl amine (83 mg, 0.83 mmol, 12 eq) was added to mixture. The reaction mixture was stirred at −78° C. for 2 hours, and then was quenched with aqueous ammonium chloride solution. The resulting mixture was extracted with ethyl acetate (2×20 mL). The combined organic layers were washed with water (5 mL), brine (5 mL), then dried over MgSO4, filtered, and evaporated under reduced pressure to give crude product, which was purified by reverse phase prep HPLC to give the title compound. MH+=349.0.

後処理

  1. stirringThe reaction mixture was stirred at −78° C. for 2 hours
  2. customwas quenched with aqueous ammonium chloride solution
  3. extractionThe resulting mixture was extracted with ethyl acetate (2×20 mL)
  4. washThe combined organic layers were washed with water (5 mL), brine (5 mL)
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customto give crude product, which
  9. customwas purified by reverse phase prep HPLC

出典と根拠

ORDレコード
ord-fbd5ed30ca9d46e493e77d39c393e159
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08710048B2

反応ノート

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