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1,2-Dichloroethane → HCID 136052169, 화합물

HRID 884637
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HRID 884637 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:13][C:12](=[O:14])[N:11]=[C:10]([C:15]3[CH:20]=[CH:19][C:18]([OH:21])=[C:17]([CH3:22])[CH:16]=3)[CH:9]=2)=[C:4]([CH3:23])[CH:3]=1.ClCCCl.C([N:35]1[CH2:40][CH2:39][CH:38]([CH:41]=O)[CH2:37][CH2:36]1)(OC(C)(C)C)=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(O)(=O)C>[OH:21][C:18]1[CH:19]=[CH:20][C:15]([C:10]2[CH:9]=[C:8]([C:5]3[CH:6]=[CH:7][C:2]([NH:1][CH2:41][CH:38]4[CH2:39][CH2:40][NH:35][CH2:36][CH2:37]4)=[CH:3][C:4]=3[CH3:23])[NH:13][C:12](=[O:14])[N:11]=2)=[CH:16][C:17]=1[CH3:22]
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참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 1514430tert-Butyl 4-formylpiperidine-1-carboxylateHCID 5049666Sodium triacetoxyborohydrideHCID 136348330HCID 136348330, 화합물

생성물 1

HCID 136052169HCID 136052169, 화합물수율 59%

시약·촉매·용매 1

HCID 176
Acetic Acid
용매

실험 절차

In a round bottom flask was added 6-(4-amino-2-methylphenyl)-4-(4-hydroxy-3-methylphenyl)pyrimidin-2(1H)-one (3) (30 mg, 0.10 mmol), 1,2 dichloroethane (2.0 mL), acetic acid (0.1 mL), and commercially available N-Boc-4-formyl piperidine (29 uL, 0.14 mmol). The reaction was stirred at room temperature for 15 minutes before adding sodium triacetoxy borohydride (30 mg, 0.14 mmol). Stirring was continued at room temperature overnight. The reaction was then quenched with saturated NaHCO3, extracted with EtOAc, dried over Na2SO4 and concentrated to dryness. The resultant oil was then dissolved in 4N HCl/dioxane (1.0 mL) and allowed to sit at RT for 30 min. or until Boc deprotection was complete. The 4N HCl/dioxane was decanted, and the residual solid product was rinsed with EtOAc 4×. The resulting orange solid was then dissolved in MeOH and purified by preparatory HPLC (5-85% gradient of AmAc/ACN, 15 min.) to give the product 4-(4-hydroxy-3-methylphenyl)-6-{2-methyl-4-[(piperidin-4 ylmethyl)amino]phenyl}pyrimidin-2(1H)-one as the acetate salt after lyopholyzation (24 mg, 59% yield).

후처리

  1. stirringStirring
  2. waitwas continued at room temperature overnight
  3. customThe reaction was then quenched with saturated NaHCO3
  4. extractionextracted with EtOAc
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated to dryness
  7. dissolutionThe resultant oil was then dissolved in 4N HCl/dioxane (1.0 mL)
  8. waitto sit at RT for 30 min. or until Boc deprotection
  9. customThe 4N HCl/dioxane was decanted
  10. washthe residual solid product was rinsed with EtOAc 4×
  11. dissolutionThe resulting orange solid was then dissolved in MeOH
  12. custompurified by preparatory HPLC (5-85% gradient of AmAc/ACN, 15 min.)

출처 및 근거

ORD 기록
ord-8e30a45119784808872d613d26f1acfa
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08242129B2

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