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

HRID 1664796
ノート
印刷プレビュー

反応式

HRID 1664796 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 67439261HCID 67439261、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-efe9ab24a9e94a77b8b5ea65a5bc0c6b
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039460B2

反応ノート

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