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Triphenylphosphine → 4-(S)-(t-butoxycarbonylamino)-1-(trifluoroacetyl)3-oxo-1,2-diazolidine

HRID 2291388
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HRID 2291388 반응식
[F:1][C:2]([F:21])([F:20])[C:3]([N:5]([C:7](=O)[C@H:8]([CH2:17][OH:18])[NH:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[NH2:6])=[O:4].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[C:13]([O:12][C:10]([NH:9][C@H:8]1[CH2:7][N:5]([C:3](=[O:4])[C:2]([F:21])([F:20])[F:1])[NH:6][C:17]1=[O:18])=[O:11])([CH3:16])([CH3:15])[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 131715808HCID 131715808, 화합물

생성물 1

HCID 147894614-(S)-(t-butoxycarbonylamino)-1-(trifluoroacetyl)3-oxo-1,2-diazolidine수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

N-(t-Butoxycarbonyl) (L)-serine trifluoroacetyl hydrazide (3.78 g, 12 mmol) and triphenylphosphine (3.46 g, 13.2 mmol) were dissolved in THF (50 ml). To the solution was added a THF solution (10 ml) of 95% diethyl azodicarboxylate (2.42 g, 2.19 ml, 13.2 mmol). The resultant mixture was stirred at room temperature for six hours and then the solvent was removed in vacuo. The residue was dissolved in ethyl acetate (100 ml) and then the solution was washed with aqueous sodium bicarbonate solution (33 ml, 3×). The sodium bicarbonate extracts were combined, aqueous saturated brine solution (70 ml) was added and the resultant mixture was extracted with ethyl acetate (120 ml, 3×). The sodium bicarbonate solution was then layered with additional ethyl acetate (200 ml) and 1N hydrochloric acid (approx. 80 ml) was added until the sodium bicarbonate solution had a pH of 2.5. The ethyl acetate layer was separated and the aqueous layer was extracted with additional ethyl acetate (4×, 125 ml). The ethyl acetate extracts were combined, washed with saturated aqueous brine (125 ml, 2×), dried over sodium sulfate, filtered, and taken to dryness in vacuo. The resultant residue was dissolved in acetonitrile (100 ml) then the acetonitrile was removed in vacuo. Treatment of the residue with acetonitrile was repeated to yield 3.06 g, 96% yield of 4-(S)-(t-butoxycarbonylamino)-1-(trifluoroacetyl)-3-oxo-1,2-diazolidine: n.m.r (300 MHz, CDCl3): δ 5.25 (d, 1, J=6), 4.81 (t, 1), 4.6 (m, 1), 4.06 (t, 1), 1.46 (s, 9); i.r. (CHCl3): 1722, 1682, 1518 cm-1 ; f.d.m.s. (m/e): M+ =297; specific rotation: [α]D25 =-88.14° (10.03 mg/ml in methanol);

후처리

  1. customthe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate (100 ml)
  3. washthe solution was washed with aqueous sodium bicarbonate solution (33 ml, 3×)
  4. additionaqueous saturated brine solution (70 ml) was added
  5. extractionthe resultant mixture was extracted with ethyl acetate (120 ml, 3×)
  6. additionwas added until the sodium bicarbonate solution
  7. customThe ethyl acetate layer was separated
  8. extractionthe aqueous layer was extracted with additional ethyl acetate (4×, 125 ml)
  9. washwashed with saturated aqueous brine (125 ml, 2×)
  10. dry with materialdried over sodium sulfate
  11. filtrationfiltered
  12. dissolutionThe resultant residue was dissolved in acetonitrile (100 ml)
  13. customthe acetonitrile was removed in vacuo

출처 및 근거

ORD 기록
ord-ed6b3ba86dca42f0bf62708db910961b
출처 데이터셋
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04795815

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