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tert-Butyl bromoacetate → Benzyl 4-(2-oxo-1,3-diazinan-1-yl)piperidine-1-carboxylate

HRID 1278985
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HRID 1278985 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([N:17]2[CH2:22][CH2:21][CH2:20][N:19](CC(O)=O)[C:18]2=[O:27])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].BrCC(OC(C)(C)C)=O>O1CCCC1.ClCCl.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:1]([O:8][C:9]([N:11]1[CH2:12][CH2:13][CH:14]([N:17]2[CH2:22][CH2:21][CH2:20][NH:19][C:18]2=[O:27])[CH2:15][CH2:16]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 79177tert-Butyl bromoacetate2회HCID 22137504[3-{1-[(Benzyloxy)carbonyl]piperidin-4-yl}-2-oxotetrahydropyrimidin-1(2H)-yl]acetic acidHCID 23665647Potassium tert-butoxide2회

생성물 1

HCID 22137530Benzyl 4-(2-oxo-1,3-diazinan-1-yl)piperidine-1-carboxylate

시약·촉매·용매 3

HCID 67553Tetrabutylammonium Iodide
촉매
HCID 6344Dichloromethane용매2회
HCID 8028Tetrahydrofuran용매

실험 절차

1-Benzyloxycarbonyl-4-(3-carboxymethyl-2-oxoperhydropyrimidin-1-yl)piperidine. Potassium tert-butoxide (52 mL, 1 M in tert-butanol) was added to l-benzyloxycarbonyl-4-(2-oxoperhydropyrimidin-1-yl)piperidine (15.0 g), and the solution was stirred for 35 minutes. tert-Butyl bromoacetate (7.65 mL) was then added, and the mixture was stirred overnight. The reaction mixture was diluted with tetrahydrofuran (20 mL) and dichloromethane (10 mL) followed by the addition of tetrabutylammonium iodide (1.74 g), potassium tert-butoxide (52 mL, 1 M in tert-butanol), and tert-butyl bromoacetate (7.65 mL). After being stirred overnight, the reaction mixture was diluted with dichloromethane and washed with water. The separated organic layer was dried, evaporated to an oil, and dissolved in 1 N hydrochloric acid (700 mL), tetrahydrofuran (200 mL), and methanol (200 mL). After being stirred overnight, the reaction mixture was concentrated in vacuo to remove the organic solvents. The resulting aqueous solution was extracted with dichloromethane, acidified with 2 N hydrochloric acid to a pH of 2, and extracted with dichloromethane. The first organic extract was concentrated to give unreacted 1-benzyloxycarbonyl-4-(2-oxoperhydropyrimidin-1-yl)piperidine (7.0 g). The second organic extract was washed with water, dried, and evaporated. The crude product was triturated from ether and filtered to give the title compound as a white solid (8.3 g); MS: m/z=376(M+1); NMR (CDCl3): 7.35 (m,5), 5.12 (s,2), 4.48 (m,1), 4.28 (m,2), 4.02 (s,2), 3.35 (m,2), 3.18 (m,2), 2.87 (m,2), 1.97 (m,2), 1.65 (m,4).

후처리

  1. stirringthe mixture was stirred overnight
  2. stirringAfter being stirred overnight
  3. washwashed with water
  4. customThe separated organic layer was dried
  5. customevaporated to an oil
  6. dissolutiondissolved in 1 N hydrochloric acid (700 mL)
  7. stirringAfter being stirred overnight
  8. concentrationthe reaction mixture was concentrated in vacuo
  9. customto remove the organic solvents
  10. extractionThe resulting aqueous solution was extracted with dichloromethane
  11. extractionextracted with dichloromethane
  12. extractionThe first organic extract
  13. concentrationwas concentrated

출처 및 근거

ORD 기록
ord-beeb88cae8ed471ea3d3070d044a5d3d
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06444809B1

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