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Water → HCID 68698709, 화합물

HRID 1990884
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HRID 1990884 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[O:16][C:17]3[CH:23]=[CH:22][C:21]([NH2:24])=[CH:20][C:18]=3[N:19]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH:25]1([C:29](Cl)=[O:30])[CH2:28][CH2:27][CH2:26]1.C(N(C(C)C)CC)(C)C.O>CN(C=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[O:16][C:17]3[CH:23]=[CH:22][C:21]([NH:24][C:29]([CH:25]4[CH2:28][CH2:27][CH2:26]4)=[O:30])=[CH:20][C:18]=3[N:19]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 4

HCID 962WaterHCID 78705Cyclobutanecarbonyl chlorideHCID 81531DiisopropylethylamineHCID 68695194HCID 68695194, 화합물

생성물 1

HCID 68698709HCID 68698709, 화합물수율 64%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-(5-amino-benzooxazol-2-ylamino)-piperidine-1-carboxylic acid tert-butyl ester (1.40 g, 4.21 mmol, 1.0 equiv) in anhydrous DMF (5 mL) was added cyclobutanecarbonyl chloride (0.55 g, 4.63 mmol, 1.1 equiv; commercially available) and diisopropylethylamine (1.03 mL, 1.14 g, 8.84 mmol, 2.1 equiv) and the reaction mixture stirred at rt. After 1 h, water was added (50 mL) and the water phase extracted with dichloromethane (3×50 mL). The combined organic phases were dried over MgSO4, the organic solvent removed under reduced pressure and the crude oil purified with column chromatography on silica eluting with ethyl acetate/heptane (2:1) to afford 1.1 g (64%) of the title compound. 1H NMR (300 MHz, CDCl3): δ 1.46-1.50 (m, 2H), 1.47 (s, 9H), 1.94-2.02 (m, 2H), 2.10-2.13 (m, 2H), 2.20-2.26 (m, 2H), 2.34-2.47 (m, 2H), 2.95-2.97 (m, 2H), 3.10-3.22 (m, 1H), 3.90 (br s, 1H), 4.05 (br s, 2H), 5.24 (brs, 1H), 7.14 (d, J=8.6 Hz, 1H), 7.28 (brs, 1H), 7.33 (d, J=8.6 Hz, 1H), 7.41 (brs, 1H). 13C NMR (75 MHz, CDCl3): δ 18.05, 25.33, 28.41, 32.30, 40.85, 42.49, 50.45, 79.76, 108.41, 108.54, 113.47, 134.57, 143.38, 145.21, 154.70, 161.76, 173.04. MS (ISP): 413.1 [M−H]−.

후처리

  1. extractionthe water phase extracted with dichloromethane (3×50 mL)
  2. dry with materialThe combined organic phases were dried over MgSO4
  3. customthe organic solvent removed under reduced pressure
  4. customthe crude oil purified with column chromatography on silica eluting with ethyl acetate/heptane (2:1)

출처 및 근거

ORD 기록
ord-739800feb7b04216aeb41dd4b7c8a3e6
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645753B2

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