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Potassium Iodide → HCID 86701104, 화합물

HRID 1396245
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HRID 1396245 반응식
[CH3:1][O:2][C:3]1[CH:36]=[CH:35][C:6]([CH2:7][O:8][C@@H:9]2[C@@H:17](/[CH:18]=[CH:19]/[O:20]C)[O:16][C@H:15]3[C@H:11]([N:12]=[C:13]([N:22]([CH3:24])[CH3:23])[S:14]3)[C@H:10]2[O:25][CH2:26][C:27]2[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=2)=[CH:5][CH:4]=1.[I-].[K+]>C(#N)C.O.[Hg](OC(C)=O)OC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][O:8][C@@H:9]2[C@@H:17]([CH2:18][CH:19]=[O:20])[O:16][C@H:15]3[C@H:11]([N:12]=[C:13]([N:22]([CH3:24])[CH3:23])[S:14]3)[C@H:10]2[O:25][CH2:26][C:27]2[CH:28]=[CH:29][C:30]([O:33][CH3:34])=[CH:31][CH:32]=2)=[CH:35][CH:36]=1
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참가 물질

6

반응물 2

HCID 4875Potassium IodideHCID 69082734HCID 69082734, 화합물

생성물 1

HCID 86701104HCID 86701104, 화합물

시약·촉매·용매 3

HCID 16683746Diacetyloxymercury촉매HCID 962Water용매2회HCID 6342Acetonitrile용매

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온도
0 °C

실험 절차

To a cold solution of 37 (100 mg, 0.18 mmol) in acetonitrile (20 mL) at −5° C. was added a solution of Hg(OAc)2 (68 mg, 0.21 mmol) in water (10 mL) dropwise. After stirred at 0° C. for 4 h, the reaction mixture was treated with potassium iodide (40 mg, 0.24 mmol) in water (1.6 mL) for 10 min. The reaction solution was quenched with water, extracted with dichloromethane (40 mL), and dried over MgSO4. Removal of solvents gave crude 2-((3aR,5R,6R,7R,7aR)-6,7-bis(4-methoxybenzyloxy)-2-(dimethylamino)-5,6,7,7a-tetrahydro-3aH-pyrano[3,2-d]thiazol-5-yl)acetaldehyde. To a solution of the crude product in dry THF (20 mL) was added NaBH4 (16 mg, 0.42 mmol) at 0° C. in portions. After stirred at 0° C. overnight, the reaction solution was quenched with water (25 mL) and extracted with ethyl acetate (2×20 mL). The combined organic phases were washed with saturated aqueous NH4Cl, dried over MgSO4, and concentrated to give a residue, which was purified by silica gel chromatography, eluted with 20-50% ethyl acetate in petroleum ether to give the product 38 as a light yellow oil (50 mg, 48%). (ES, m/z)[M+H]+ 503.0; 1H NMR (300 MHz, CDCl3) δ 7.15-7.35 (m, 4H), 6.84-6.98 (m, 4H), 6.28 (d, J=6.3 Hz, 1H), 4.45-4.89 (m, 4H), 4.18 (t, J=5.7 Hz, 1H), 3.94 (t, J=4.8 Hz, 1H), 3.87-3.91 (m, 1H), 3.78 (s, 6H), 3.56-3.65 (m, 3H), 2.92 (s, 6H), 1.89-1.98 (m, 1H), 1.62-1.73 (m, 1H).

후처리

  1. customThe reaction solution was quenched with water
  2. extractionextracted with dichloromethane (40 mL)
  3. dry with materialdried over MgSO4
  4. customRemoval of solvents

출처 및 근거

ORD 기록
ord-42999f579a804fa287d6a22c29ac842a
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901087B2

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