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Benzyl Chloride → (S)-4-tert-Butoxycarbonylamino-5-methyl-hexanoic acid, benzyl ester

HRID 1968783
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HRID 1968783 반응식
[C:1]([O:5][C:6]([NH:8][C@H:9]([CH:15]([CH3:17])[CH3:16])[CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:24](Cl)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(=O)(O)[O-].[Na+]>CCCCCCC.ClCCl.O1CCCC1>[C:1]([O:5][C:6]([NH:8][C@H:9]([CH:15]([CH3:17])[CH3:16])[CH2:10][CH2:11][C:12]([O:14][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:13])=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7503Benzyl ChlorideHCID 10796Cesium carbonateHCID 516892Sodium BicarbonateHCID 57678353(4S)-4-{[(tert-butoxy)carbonyl]amino}-5-methylhexanoic acid

생성물 1

HCID 58625169(S)-4-tert-Butoxycarbonylamino-5-methyl-hexanoic acid, benzyl ester

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 21907733Dichloromethane heptane용매

실험 절차

A 50 mL, one-neck round bottom flask (equipped with a magnetic stirrer and a nitrogen inlet) was charged with (S)-4-tert-butoxycarbonylamino-5-methyl-hexanoic acid prepared as in Example 63 above (500 mg, 2.04 mmol), cesium carbonate (1.99 g, 6.11 mmol), benzyl chloride (773 mg, 6.11 mmol), and tetrahydrofuran (15 mL). The reaction was stirred at room temperature for three days (weekend) and then was heated to a mild reflux for 6 h. The reaction mixture was poured into saturated aqueous sodium bicarbonate (100 mL) and extracted with ethyl ether (2×100 mL). The combined organics were dried and concentrated to give 1 g of crude product. The residue was dissolved in heptane-dichloromethane (9:1, ˜7 mL) and eluted through a 12 g Isco silica gel cartridge to yield the title compound as a solid.

후처리

  1. customA 50 mL, one-neck round bottom flask (equipped with a magnetic stirrer and a nitrogen inlet)
  2. temperaturewas heated to
  3. temperaturea mild reflux for 6 h
  4. extractionextracted with ethyl ether (2×100 mL)
  5. customThe combined organics were dried
  6. concentrationconcentrated
  7. customto give 1 g of crude product
  8. washeluted through a 12 g Isco silica gel cartridge

출처 및 근거

ORD 기록
ord-33953d1b872143618c02174597753380
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08426429B2

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