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Triethylamine → (R)-3-(N-(tert-butoxycarbonyl)glycyl)amino-1-(4-chlorobenzyl)pyrrolidine

HRID 133554
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HRID 133554 반응식
[NH2:1][C@@H:2]1[CH2:6][CH2:5][N:4]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[CH2:3]1.C(N(CC)CC)C.[C:22]([O:26][C:27]([NH:29][CH2:30][C:31](O)=[O:32])=[O:28])([CH3:25])([CH3:24])[CH3:23].CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[OH-].[Na+]>ClCCl>[C:22]([O:26][C:27]([NH:29][CH2:30][C:31]([NH:1][C@@H:2]1[CH2:6][CH2:5][N:4]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[CH2:3]1)=[O:32])=[O:28])([CH3:25])([CH3:24])[CH3:23]
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참가 물질

8

반응물 6

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 78288N-(tert-butoxycarbonyl)glycineHCID 24904911(R)-3-amino-1-(4-chlorobenzyl)pyrrolidine

생성물 1

HCID 53939240
(R)-3-(N-(tert-butoxycarbonyl)glycyl)amino-1-(4-chlorobenzyl)pyrrolidine
수율 92%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

To a dichloromethane (80 mL) solution of the (R)-3-amino-1-(4-chlorobenzyl)pyrrolidine (3.35 g, 16 mmol), were added triethylamine (2.5 mL, 17.6 mmol), N-tert-butoxycarbonylglycine (2.79 g, 16.0 mmol), EDCI (3.07 g, 16.0 mmol) and HOBt (12.16 g, 16 mmol). The resulting reaction mixture was stirred at 25° C. for 16 hours, and a 2 M solution (80 mL) of NaOH was then added thereto. The organic layer was separated, and the aqueous layer was extracted with dichloromethane (100 mL×3). The organic layers were combined, washed with water (100 mL×2) and brine (100 mL), dried over anhydrous sodium sulfate, filtered, concentrated and purified by column chromatography (SiO2, ethyl acetate) to thereby provide the objective (R)-3-[N-(tert-butoxycarbonyl)glycyl]amino-1-(4-chlorobenzyl)pyrrolidine (5.40 g, 92%).

후처리

  1. customThe resulting reaction mixture
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with dichloromethane (100 mL×3)
  4. washwashed with water (100 mL×2) and brine (100 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. custompurified by column chromatography (SiO2, ethyl acetate)

출처 및 근거

ORD 기록
ord-102766b4e31e467aab5aee47b5408347
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07390830B1

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