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Triethylamine → HCID 86658429, 화합물

HRID 1968879
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HRID 1968879 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C@@H:7]1[CH2:9][C@H:8]1[C:10]([OH:12])=O.C(Cl)(=O)C(Cl)=O.[Si:19]([O:26][C:27]1[CH:32]=[CH:31][C:30]([NH:33][CH2:34][C@@H:35]([NH:40][C:41](=[O:47])[O:42][C:43]([CH3:46])([CH3:45])[CH3:44])[C@@H:36]([CH3:39])[CH2:37][CH3:38])=[CH:29][CH:28]=1)([C:22]([CH3:25])([CH3:24])[CH3:23])([CH3:21])[CH3:20].C(N(CC)CC)C>CN(C=O)C.C(OCC)C.ClCCl>[Si:19]([O:26][C:27]1[CH:32]=[CH:31][C:30]([N:33]([CH2:34][C@@H:35]([NH:40][C:41](=[O:47])[O:42][C:43]([CH3:44])([CH3:46])[CH3:45])[C@@H:36]([CH3:39])[CH2:37][CH3:38])[C:10]([C@@H:8]2[CH2:9][C@H:7]2[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)=[O:12])=[CH:29][CH:28]=1)([C:22]([CH3:23])([CH3:24])[CH3:25])([CH3:21])[CH3:20]
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참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 39235822rac-(1R,2R)-2-(pyridin-2-yl)cyclopropane-1-carboxylic acidHCID 67114485HCID 67114485, 화합물

생성물 1

HCID 86658429HCID 86658429, 화합물수율 77%

시약·촉매·용매 3

HCID 6228
Dimethylformamide
촉매
HCID 3283Diethyl Ether용매
HCID 6344Dichloromethane용매

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온도
35 °C

실험 절차

A solution of trans-2-pyridin-2-yl-cyclopropylcarboxylic acid (270 mg, 1.7 mmol) and dichloromethane (15 mL) was treated with oxalyl chloride (170 μL, 2.0 mmol) and DMF (1 drop). The resulting reaction mixture was maintained at 35° C. for 3 h, then concentrated under reduced pressure to dryness. The residue was dissolved in dichloromethane (15 mL), and treated with tert-butyl (2S,3S)-1-(4-(tert-butyldimethylsilyloxy)phenylamino)-3-methylpentan-2-ylcarbamate (700 mg, 1.7 mmol) and triethylamine (690 μL, 5.0 mmol). The reaction mixture was maintained at room temperature overnight, then diluted with diethyl ether (30 mL) washed with saturated aqueous sodium bicarbonate (30 mL) and brine (30 mL), then dried over MgSO4, filtered and concentrated to afford a residue that was purified by column chromatography on silica gel (eluting with 15% ethyl acetate in hexanes) to afford tert-butyl (2S,3S)-1-(N-(4-(tert-butyldimethylsilyloxy)phenyl)-trans-2-(pyridin-2-yl)cyclopropanecarboxamido)-3-methylpentan-2-ylcarbamate (720 mg, 77% yield) as a yellow oil: 1H NMR (400 MHz, CDCl3) δ 8.04-8.13 (m, 1H), 7.25-7.36 (m, 1H), 6.91-7.00 (m, 1H), 6.87-6.91 (m, 1H), 6.76-6.86 (m, 2H), 6.55-6.62 (m, 1H), 6.46-6.55 (m, 1H), 4.83-4.98 (m, 1H), 4.15-4.27 (m, 1H), 3.45-3.64 (m, 1H), 2.81-2.93 (m, 1H), 2.23-2.48 (m, 1H), 1.68-1.81 (m, 1H), 1.37 (s, 3H), 1.29-1.52 (m, 2H), 1.28 (s, 3H), 1.25 (s, 3H), 1.15-1.22 (m, 1H), 0.86-0.97 (m, 1H), 0.78 (d, J=5.1 Hz, 9H), 0.67-0.71 (m, 3H), 0.60-0.67 (m, 3H), −0.06-0.02 (m, 6H); LRMS (ESI) m/e 568.3 [(M+H)+, calcd for C32H50N3O4Si 568.3].

후처리

  1. customThe resulting reaction mixture
  2. concentrationconcentrated under reduced pressure to dryness
  3. dissolutionThe residue was dissolved in dichloromethane (15 mL)
  4. temperatureThe reaction mixture was maintained at room temperature overnight
  5. washwashed with saturated aqueous sodium bicarbonate (30 mL) and brine (30 mL)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto afford a residue that
  10. customwas purified by column chromatography on silica gel (eluting with 15% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-0c4d1bd6ef6a4990b11f161f7e1d3d5c
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08426414B2

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