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tert-Butyl acetate → Tert-butyl (S)-4-(cbz-amino)-5-methyl-3-oxohexanoate

HRID 1585778
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HRID 1585778 반응식
[CH3:1][CH:2]([C@H:4]([NH:8][C:9]([O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:10])[C:5]([OH:7])=O)[CH3:3].[C:19]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])(=[O:21])[CH3:20].[Li+].CC([N-]C(C)C)C.[N-]1C=CN=C1>O1CCCC1>[C:23]([O:22][C:19](=[O:21])[CH2:20][C:5](=[O:7])[C@@H:4]([NH:8][C:9]([O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:10])[CH:2]([CH3:1])[CH3:3])([CH3:26])([CH3:25])[CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 10908tert-Butyl acetateHCID 726987N-Carbobenzoxy-L-valineHCID 2724682Lithium diisopropylamideHCID 3386966Imidazolate

생성물 1

HCID 11221808Tert-butyl (S)-4-(cbz-amino)-5-methyl-3-oxohexanoate수율 98.9%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

To an ice-cooled solution of Z-valine (5 g, 19.9 mmol) in 60 ml tetrahydrofurane was added N,N'-cabonyldiimidazole (3.55 g, 22.3 mmol) in one portion and stirred for 3 h. At -78° C., tert-butyl acetate (13.5 ml, 100 mmol) was dropped to a solution of LDA (90 mmol) in tetrahydrofurane (270 ml). After 30', the imidazolide solution was added dropwise via double-ended needle to the enolate. The resulting mixture was stirred for 2 h until the temperature rose to -15° C. The reaction was quenched with 400 ml saturated aqueous NH4Cl and extracted with ether (3×200 ml). The combined organic extracts were washed with 2N aqueous HCl (50 ml), saturated aqueous NaHCO3 (2×50 ml), dried over magnesium sulfate and evaporated to dryness in vacuo. The residue was purified by column chromatography on silica gel using ethyl acetate-hexane (1:4) as an eluent to give the product as a colorless oil (6.88 g)

후처리

  1. stirringThe resulting mixture was stirred for 2 h until the temperature
  2. customrose to -15° C
  3. customThe reaction was quenched with 400 ml saturated aqueous NH4Cl
  4. extractionextracted with ether (3×200 ml)
  5. washThe combined organic extracts were washed with 2N aqueous HCl (50 ml), saturated aqueous NaHCO3 (2×50 ml)
  6. dry with materialdried over magnesium sulfate
  7. customevaporated to dryness in vacuo
  8. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-1a09c79c28e34a33bfdf04e86e126d18
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05939527

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