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Acetic Acid → tert-Butyl 4-[4-(1H-tetrazol-1-yl)anilino]-1-piperidinecarboxylate

HRID 412900
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HRID 412900 반응식
[N:1]1([C:6]2[CH:12]=[CH:11][C:9]([NH2:10])=[CH:8][CH:7]=2)[CH:5]=[N:4][N:3]=[N:2]1.[C:13]([O:17][C:18]([N:20]1[CH2:25][CH2:24][C:23](=O)[CH2:22][CH2:21]1)=[O:19])([CH3:16])([CH3:15])[CH3:14].C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>C1COCC1>[N:1]1([C:6]2[CH:12]=[CH:11][C:9]([NH:10][CH:23]3[CH2:24][CH2:25][N:20]([C:18]([O:17][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:19])[CH2:21][CH2:22]3)=[CH:8][CH:7]=2)[CH:5]=[N:4][N:3]=[N:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 5716404-(1H-1,2,3,4-tetrazol-1-yl)anilineHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 5049666Sodium triacetoxyborohydride2회

생성물 1

HCID 18539221tert-Butyl 4-[4-(1H-tetrazol-1-yl)anilino]-1-piperidinecarboxylate
수율 98.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-(1H-tetrazol-1-yl)aniline (2 g, 12.4 mmol) and 1-tert-butoxycarbonyl-4-piperidone (3.71 g, 18.6 mmol) in THF (15 ml) were added acetic acid (1.42 ml, 24.8 mmol) and sodium triacetoxyborohydride (4 g, 18.6 mmol), successively, under ice cooling, and the mixture was stirred for 20 hours. To the mixture was added sodium triacetoxyborohydride (4 g, 18.6 mmol), and the mixture was stirred at room temperature for 20 hours. To the mixture was added saturated aqueous solution of sodium hydrogencarbonate (100 ml), and the mixture was stirred at room temperature for 1 hour. The mixture was extracted with ethyl acetate (100 ml), and the organic layer was washed with saturated sodium chloride solution (50 ml), dried over anhydrous sodium sulfate and concentrated under reduced pressure. To the concentrate was added diisopropyl ether (20 ml), and the resulting precipitates were collected by filtration to give the titled compound (4.2 g).

후처리

  1. stirringthe mixture was stirred at room temperature for 20 hours
  2. stirringthe mixture was stirred at room temperature for 1 hour
  3. extractionThe mixture was extracted with ethyl acetate (100 ml)
  4. washthe organic layer was washed with saturated sodium chloride solution (50 ml)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionTo the concentrate was added diisopropyl ether (20 ml)
  8. customthe resulting precipitates
  9. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-cd2ed117637349a7baee0934ce2df531
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06562978B1

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