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HCID 67439261, 화합물 → 1-Methyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

HRID 1664796
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HRID 1664796 반응식
[CH3:1][N:2]1[C:6]2([CH2:11][CH2:10][N:9](C(OCC3C=CC=CC=3)=O)[CH2:8][CH2:7]2)[C:5](=[O:22])[NH:4][C:3]1=[O:23]>C(O)C.[Pd]>[CH3:1][N:2]1[C:6]2([CH2:7][CH2:8][NH:9][CH2:10][CH2:11]2)[C:5](=[O:22])[NH:4][C:3]1=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 67439261HCID 67439261, 화합물

생성물 1

HCID 2720021-Methyl-1,3,8-triazaspiro[4.5]decane-2,4-dione수율 66.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

Palladium (10% on carbon; 1.0 g) was added to a solution of benzyl 1-methyl-2,4-dioxo-1,3,8-triazaspiro[4.5]decane-8-carboxylate (7.82 g, 24.6 mmol) in ethanol (100 mL). The reaction vessel was evacuated and back-filled with nitrogen (3×), then back-filled with hydrogen (1 atm). After 2 h, methanol (50 mL) was added to the reaction mixture and the mixture was continued to be stirred under hydrogen (1 atm). After 4 days, the mixture was filtered through celite, washed with acetone and concentrated. The mixture was diluted in acetic acid (50 mL). The reaction vessel was evacuated and back-filled with nitrogen (3×), then back-filled with hydrogen (1 atm). After 2 h, the mixture was filtered through celite, and concentrated to give the acetate salt of the title compound (2.98 g). MS 184.1 (M+1).

후처리

  1. customThe reaction vessel was evacuated
  2. additionback-filled with nitrogen (3×)
  3. additionback-filled with hydrogen (1 atm)
  4. additionmethanol (50 mL) was added to the reaction mixture
  5. waitAfter 4 days
  6. filtrationthe mixture was filtered through celite
  7. washwashed with acetone
  8. concentrationconcentrated
  9. additionThe mixture was diluted in acetic acid (50 mL)
  10. customThe reaction vessel was evacuated
  11. additionback-filled with nitrogen (3×)
  12. additionback-filled with hydrogen (1 atm)
  13. waitAfter 2 h
  14. filtrationthe mixture was filtered through celite
  15. concentrationconcentrated

출처 및 근거

ORD 기록
ord-efe9ab24a9e94a77b8b5ea65a5bc0c6b
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08039460B2

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