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1-Hydroxybenzotriazole → (S)-2-[[(S)-2-(Acetoxyacetyl)-1-pyrrolidinyl]carbonyl]-N-(phenylmethyl)-1-pyrrolidinecarboxamide

HRID 1735391
ノート
印刷プレビュー

反応式

HRID 1735391 の反応式
[C:1]([O:4][CH2:5][C:6]([C@@H:8]1[CH2:12][CH2:11][CH2:10][N:9]1[C:13]([O:15]C(C)(C)C)=O)=[O:7])(=[O:3])[CH3:2].[NH:20]1[CH2:27][CH2:26][CH2:25][C@H:21]1C(O)=O.[CH2:28]([N:35]=[C:36]=[O:37])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.C1C=CC2N(O)N=NC=2C=1>FC(F)(F)C(O)=O.C(O)(=O)C.CN(C=O)C.C(Cl)Cl.O.C(N(CC)CC)C>[C:1]([O:4][CH2:5][C:6]([C@@H:8]1[CH2:12][CH2:11][CH2:10][N:9]1[C:13]([C@@H:27]1[CH2:26][CH2:25][CH2:21][N:20]1[C:36]([NH:35][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:37])=[O:15])=[O:7])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 76639Benzyl isocyanateHCID 145742L-ProlineHCID 13753435(S)-2-(Acetoxyacetyl)-1-(tert-butoxycarbonyl)pyrrolidine

生成物 1

HCID 15389023(S)-2-[[(S)-2-(Acetoxyacetyl)-1-pyrrolidinyl]carbonyl]-N-(phenylmethyl)-1-pyrrolidinecarboxamide収率 40.8%

試薬・触媒・溶媒 5

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 6344Dichloromethane溶媒
HCID 8471Triethylamine溶媒
HCID 23437676Trifluoroacetic acid acetate溶媒

実験手順

(S)-2-(Acetoxyacetyl)-1-(tert-butoxycarbonyl)pyrrolidine (8.9 g) was dissolved in trifluoroacetic acid-acetic acid (1:1 solution, 90 ml), and the mixture was stirred at room temperature for 1.5 hours. The reaction mixture was concentrated under reduced pressure and the residue was suspended in methylene chloride. The suspension was added to a solution of N-(benzylaminocarbonyl)-L-proline obtained by stirring L-proline (4.0 g), benzyl isocyanate (3.9 g) and triethylamine (3.5 g) in DMF (40 ml) at room temperature for 1 hour. Then, HOBt (4.7 g) and water-soluble carbodiimide hydrochloride (6.7 g) were added. The mixture was stirred at room temperature overnight and methylene chloride was added to the reaction mixture. The resulting mixture was washed with 10% potassium hydrogensulfate, a saturated aqueous solution of sodium bicarbonate and water in order, dried over anhydrous sodium sulfate, and concentrated. The residue was dissolved in ethyl acetate, added with active charcoal, stirred at room temperature for 30 minutes, filtered and concentrated to give the title compound (4.8 g) (see Table 1).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionThe suspension was added to a solution of N-(benzylaminocarbonyl)-L-proline
  3. customobtained
  4. stirringThe mixture was stirred at room temperature overnight
  5. washThe resulting mixture was washed with 10% potassium hydrogensulfate
  6. dry with materiala saturated aqueous solution of sodium bicarbonate and water in order, dried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. dissolutionThe residue was dissolved in ethyl acetate
  9. additionadded with active charcoal
  10. stirringstirred at room temperature for 30 minutes
  11. filtrationfiltered
  12. concentrationconcentrated

出典と根拠

ORDレコード
ord-a356c5e06f984e8cb39c8958c1b4eb45
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05536737

反応ノート

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