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

HRID 1988415
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HRID 1988415 반응식
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
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참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 57725827HCID 57725827, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e797f3f454dc4cf8a08df4e2df2ff3aa
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07553854B2

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