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Tetrahydrofuran → HCID 68090528, 화합물

HRID 1882352
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HRID 1882352 반응식
[C:1]([O:5][C:6]([NH:8][C:9]1[S:10][C:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:12]([CH3:14])[N:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:20][C@@H:21]([CH3:24])[CH2:22]O.C1(P([C:38]2[CH:43]=[CH:42]C=CC=2)C2C=CC=CN=2)C=CC=CC=1.N(C(OCC)=O)=N[C:46]([O:48]CC)=[O:47].O1CCC[CH2:57]1>C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]([CH2:22][C@@H:21]([NH:20][C:46]([O:48][C:43]([CH3:42])([CH3:38])[CH3:57])=[O:47])[CH3:24])[C:9]1[S:10][C:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:12]([CH3:14])[N:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

7

반응물 5

HCID 8028TetrahydrofuranHCID 80307L-AlaninolHCID 220568ethyl N-ethoxycarbonyliminocarbamate2회HCID 6218932-Pyridyldiphenylphosphine2회HCID 53404548Ethyl 2-(tert-butoxycarbonylamino)-4-methylthiazole-5-carboxylate

생성물 1

HCID 68090528HCID 68090528, 화합물
수율 78%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of ethyl 2-(tert-butoxycarbonylamino)-4-methylthiazole-5-carboxylate (0.29 g, 1.00 mmol), (S)-(+)-2-amino-1-propanol (0.18 g, 1.00 mmol) and diphenyl-2-pyridinylphosphine (0.40 g, 1.50 mmol) in anhydrous tetrahydrofuran (20.0 mL) was added diethyl azodicarboxylate (0.26 g, 1.50 mmol) at 0° C. The resulting solution was stirred at ambient temperature for 0.5 h. Additional diphenyl-2-pyridinylphosphine (0.13 g, 0.50 mmol) and diethyl azodicarboxylate (0.096 g, 0.50 mmol) were added to the reaction mixture and stirred at ambient temperature for 4 h. The reaction mixture was diluted with ethyl acetate (80 mL) and washed with 25% aqueous ammonium chloride solution (3×20 mL). The organic layer was dried over anhydrous sodium sulphate and filtered. The filtrate was concentrated in vacuo and the residue was purified by column chromatography eluted with 15-45% ethyl acetate in hexanes to afford the title compound as a colorless oil (0.35 g, 78%): 1H NMR (300 MHz, CDCl3) δ 5.30 (s, 1H), 4.26 (q, J=7.1 Hz, 2H), 4.18-3.95 (m, 3H), 2.59 (s, 3H), 1.58 (s, 9H), 1.33-1.28 (m, 12H), 1.17 (d, J=6.3 Hz, 3H); MS (ES+) m/z 244 (M−2Boc+1).

후처리

  1. stirringstirred at ambient temperature for 4 h
  2. washwashed with 25% aqueous ammonium chloride solution (3×20 mL)
  3. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue was purified by column chromatography
  7. washeluted with 15-45% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-de02c2c8ed4e411abb275ea9acaee07b
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318949B2

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