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Hydrochloric Acid → HCID 66673584, 화합물

HRID 423686
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HRID 423686 반응식
Cl.[CH3:2][S:3]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:17]=[CH:16][C:15]([O:18][CH2:19][CH:20]3[CH2:25][CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22][CH2:21]3)=[CH:14][CH:13]=2)=[CH:8][CH:7]=1)(=[O:5])=[O:4].[C:33]([OH:39])([C:35]([F:38])([F:37])[F:36])=[O:34]>O1CCOCC1>[C:33]([OH:39])([C:35]([F:38])([F:37])[F:36])=[O:34].[F:36][C:35]([F:38])([F:37])[C:33]([OH:39])=[O:34].[CH3:2][S:3]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:13]=[CH:14][C:15]([O:18][CH2:19][CH:20]3[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]3)=[CH:16][N:17]=2)=[CH:8][CH:7]=1)(=[O:4])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 6422Trifluoroacetic acidHCID 249943331,1-Dimethylethyl 4-[({6-[4-(methylsulfonyl)phenyl]-3-pyridinyl}oxy)methyl]-1-piperidinecarboxylate

생성물 2

HCID 6422Trifluoroacetic acid수율 0.05%HCID 66673584HCID 66673584, 화합물수율 23%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매3회

실험 절차

4N HCl in 1,4-dioxane (1 mL) was added to a mixture of 1,1-dimethylethyl 4-[({6-[4-(methylsulfonyl)phenyl]-3-pyridinyl}oxy)methyl]-1-piperidinecarboxylate (462 mg, 1.03 mmol) in 1,4-dioxane (10 mL) at ambient temperature. The mixture was stirred at ambient temperature overnight. The mixture was charged with additional 4N HCl in 1,4-dioxane (1 mL), and stirred at ambient temperature overnight. The mixture was then charged with TFA (2 mL), and stirred at ambient temperature for 4 h. The mixture was concentrated, diluted with water, basified with saturated NaHCO3, and extracted with EtOAc. The organics were dried over MgSO4, filtered, and the filtrate was concentrated. The crude product was purified by reverse-phase preparative HPLC using CH3CN:H2O gradient (5:95 to 75:25) with 0.05% TFA as a modifier to give 107 mg (23%) of 2-[4-(methylsulfonyl)phenyl]-5-[(4-piperidinylmethyl)oxy]pyridine trifluoroacetate as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 8.59-8.50 (m, 1H), 8.44 (d, 1H, J=2.9 Hz), 8.28 (d, 2H, J=8.6 Hz), 8.08 (d, 1H, J=8.8 Hz), 8.00 (d, 2H, J=8.6 Hz), 7.55 (dd, 1H, Ja=8.8 Hz, Jb=3.0 Hz), 4.04 (d, 2H, J=6.2 Hz), 3.40-3.25 (m, 2H), 3.25 (s, 3H), 3.00-2.86 (m, 2H), 2.16-2.06 (m, 1H), 2.05-1.90 (m, 2H), 1.56-1.40 (m, 2H); LRMS (ESI), m/z 347 (M+H).

후처리

  1. stirringstirred at ambient temperature overnight
  2. stirringstirred at ambient temperature for 4 h
  3. concentrationThe mixture was concentrated
  4. additiondiluted with water
  5. extractionextracted with EtOAc
  6. dry with materialThe organics were dried over MgSO4
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated
  9. customThe crude product was purified by reverse-phase preparative HPLC

출처 및 근거

ORD 기록
ord-0beba2f7ad08408a9e9aafb117a82153
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101634B2

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