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Pyridine → HCID 57741115, 화합물

HRID 1092433
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HRID 1092433 반응식
[CH3:1][C:2]([O:4][C:5]([CH3:7])=[O:6])=O.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([C@@H:15]2[C@@H:20]([OH:21])[C@H](CO)[C@@H:18]([OH:24])[C@H:17]([OH:25])[C@H:16]2[OH:26])=[CH:11][C:10]=1[CH2:27][C:28]1[CH:33]=[CH:32][C:31]([CH2:34][CH3:35])=[CH:30][CH:29]=1.N1C=CC=CC=1>CN(C1C=CN=CC=1)C.C(Cl)Cl>[C:5]([O:4][CH2:2][C@@H:1]1[C@@H:18]([OH:24])[C@H:17]([OH:25])[C@@H:16]([OH:26])[C@H:15]([C:12]2[CH:13]=[CH:14][C:9]([Cl:8])=[C:10]([CH2:27][C:28]3[CH:29]=[CH:30][C:31]([CH2:34][CH3:35])=[CH:32][CH:33]=3)[CH:11]=2)[C@H:20]1[OH:21])(=[O:6])[CH3:7]
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참가 물질

6

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 42622954HCID 42622954, 화합물

생성물 1

HCID 57741115HCID 57741115, 화합물수율 50.4%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane
용매

실험 절차

Ac2O (377 mg, 1.5 eq) was added dropwised into the solution of (1R,2R,3S,4R,5R,6S)-4-(4-chloro-3-(4-ethylbenzyl)phenyl)-6-(hydroxymethyl)cyclohexane-1,2,3,5-tetraol (5, R=Et, 1 g, 2.46 mmol) and DMAP (cat.) in CH2Cl2 (10 mL) at 0° C. followed by pyridine (292 mg, 1.5 eq), and the mixture was stirred overnight at rt. The reaction mixture was washed with 3N HCl, and the organic layer was combined, dried over Na2SO4, filtered, and the filtrate was evaporated to dryness. The residue was purified by preperative HPLC to give target compound (566 mg, white solid, yield of 50.4%). 1H-NMR (400 MHz, CD3OD): δ 7.32 (1H, d, J=8.4 Hz), 7.06-7.14 (6H, m), 4.37 (2H, ddd, J=2.0, 10.8, 16.8 Hz), 4.04 (2H, s), 3.57 (1H, t, J=10.8 Hz), 3.40-3.47 (1H, m), 2.49-2.60 (3H, m), 2.04 (3H, s), 1.60-1.66 (1H, m), 1.18 (3H, t, J=8.0 Hz); MS (ESI+): 449 [M+H]+, 466 [M+NH4]+, 897 [2M+H]+, (ESI−): 492 [M+HCOO]−, 941 [2M+HCOO]−.

후처리

  1. washThe reaction mixture was washed with 3N HCl
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. customthe filtrate was evaporated to dryness
  5. customThe residue was purified by preperative HPLC
  6. customto give target compound (566 mg, white solid, yield of 50.4%)

출처 및 근거

ORD 기록
ord-3f9fbf09a3e54d60a677210f2d85d9f6
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08129434B2

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