홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Acetic Acid → 4-[2-(2,2-Dimethyl-4,6-dioxo-[1,3]dioxan-5-yl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester

HRID 899053
노트
인쇄 미리보기

반응식

HRID 899053 반응식
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=[O:5])[O:3]1.[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][CH:21]([CH2:24][CH:25]=O)[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12].C(O)(=O)C.N1CCCCC1.[BH4-].[Na+].Cl>ClCCl.COC(C)(C)C>[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][CH:21]([CH2:24][CH2:25][CH:6]2[C:7](=[O:8])[O:9][C:2]([CH3:10])([CH3:1])[O:3][C:4]2=[O:5])[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 8082PiperidineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 4311764Sodium borohydrideHCID 10353694tert-Butyl 4-(2-oxoethyl)piperidine-1-carboxylate

생성물 1

HCID 68508700
4-[2-(2,2-Dimethyl-4,6-dioxo-[1,3]dioxan-5-yl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester
수율 66.6%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 15413tert-Butyl methyl ether용매

반응 조건

온도
0 °C

실험 절차

To a solution of meldrums acid (1.68 g, 11.66 mmol) and 4-(2-oxo-ethyl)-piperidine-1-carboxylic acid tert-butyl ester (2.21 g, 9.72 mmol) in dichloromethane (40 mL) was added acetic acid (0.055 mL, 0.972 mmol) and piperidine (0.096 mL, 0.972 mmol). The mixture was heated at reflux for 3 h, and then allowed to attain room temperature. After being diluted with tert-butyl methyl ether, the mixture was washed with NaHCO3 (sat.) and brine. The organic phase was dried, filtered and concentrated. The residue was dissolved in a mixture of EtOH (40 mL) and acetic acid (20 mL). The solution was cooled to 0° C., and NaBH4 (0.554 g, 14.6 mmol) was added in portions after which the solution was allowed to stir for 30 min at rt and then acidified to pH 3 with 1 M HCl. The solution was extracted several times with dichloromethane. The combined organic phases were dried, filtered, concentrated and filtered through a pad of silica gel (dichloromethane). The solvent was evaporated to give 4-[2-(2,2-Dimethyl-4,6-dioxo-[1,3]dioxan-5-yl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester as a colorless oil (2.30 g, 65%) which solidified on standing.

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 3 h
  3. customto attain room temperature
  4. washthe mixture was washed with NaHCO3 (sat.) and brine
  5. customThe organic phase was dried
  6. filtrationfiltered
  7. concentrationconcentrated
  8. dissolutionThe residue was dissolved in a mixture of EtOH (40 mL) and acetic acid (20 mL)
  9. extractionThe solution was extracted several times with dichloromethane
  10. customThe combined organic phases were dried
  11. filtrationfiltered
  12. concentrationconcentrated
  13. filtrationfiltered through a pad of silica gel (dichloromethane)
  14. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-b69b2450413740f7b36a00f99004e9d2
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07354895B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트