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Hydrochloric Acid → HCID 56837183、化合物

HRID 1038301
ノート
印刷プレビュー

反応式

HRID 1038301 の反応式
[CH2:1]([O:3][C@@H:4]1[C@@H:9]([O:10][CH3:11])[C@H:8]([CH3:12])[O:7][C@@H:6]([O:13][N:14]=[CH:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]3[N:26]=[CH:25][N:24]([C:27]4[CH:32]=[CH:31][C:30]([O:33][C:34]([F:40])([F:39])[C:35]([F:38])([F:37])[F:36])=[CH:29][CH:28]=4)[N:23]=3)=[CH:18][CH:17]=2)[C@@H:5]1[O:41][CH3:42])[CH3:2].C(O)C.Cl.C(=O)(O)[O-].[Na+]>C(O)C.O>[CH2:1]([O:3][C@@H:4]1[C@@H:9]([O:10][CH3:11])[C@H:8]([CH3:12])[O:7][C@@H:6]([O:13][NH:14][CH2:15][C:16]2[CH:17]=[CH:18][C:19]([C:22]3[N:26]=[CH:25][N:24]([C:27]4[CH:32]=[CH:31][C:30]([O:33][C:34]([F:40])([F:39])[C:35]([F:37])([F:38])[F:36])=[CH:29][CH:28]=4)[N:23]=3)=[CH:20][CH:21]=2)[C@@H:5]1[O:41][CH3:42])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 516892Sodium BicarbonateHCID 866626846-Deoxy-3-O-ethyl-2,4-di-O-methyl-1-O-[(4-{1-[4-(pentafluoroethoxy)phenyl]-1H-1,2,4-triazol-3-yl}benzylidene)amino]-α-L-mannopyranose

生成物 1

HCID 56837183HCID 56837183、化合物収率 63.4%

試薬・触媒・溶媒 1

HCID 19096565
Water ethanol
溶媒

実験手順

To a solution of 4-[1-(4-pentafluoroethyloxy-phenyl)-1H-[1,2,4]triazol-3-yl]-benzaldehyde O-((2S,3R,4R,5S,6S)-4-ethoxy-3,5-dimethoxy-6-methyl-tetrahydropyran-2-yl)-oxime (P-1; 257 milligrams (mg), 0.429 millimoles (mmol)) in 190 proof ethyl alcohol (EtOH; 10 milliliters (mL)) at room temperature was added pyridine borane complex (200 microliters (μL), 1.99 mmol) in one portion. 3 N Hydrochloric acid (HCl; 1.4 mL) was then added dropwise. When the addition was complete, the mixture stirred at room temperature for 23 hours (h). The mixture was then diluted with EtOH/water (H2O) and treated with saturated sodium bicarbonate (NaHCO3). The resulting aqueous mixture was extracted with ethyl acetate (EtOAc; 2×). The organic extracts were combined, dried, washed with brine and dried with anhydrous sodium sulfate (Na2SO4). The solvent was evaporated at room temperature under vacuum. The resulting crude material was purified by silica gel chromatography (eluting with 50% EtOAc in Hexane). The title product (164 mg, 63%) was isolated as a white sticky solid: 1H NMR (300 MHz, CDCl3) δ 8.60 (s, 1H), 8.22-8.16 (m, 2H), 7.87-7.80 (m, 2H), 7.50 (d, J=8.2 Hz, 2H), 7.46-7.38 (m, 2H), 6.04 (s, 1H), 5.01 (d, J=1.4 Hz, 1H), 4.18 (s, 2H), 3.84-3.28 (m, 12H), 3.11 (dd, J=12.0, 6.5 Hz, 1H), 1.30 (ddd, J=20.9, 10.3, 4.6 Hz, 6H); ESIMS m/z 603 (M+H).

後処理

  1. additionWhen the addition
  2. extractionThe resulting aqueous mixture was extracted with ethyl acetate (EtOAc; 2×)
  3. customdried
  4. washwashed with brine
  5. dry with materialdried with anhydrous sodium sulfate (Na2SO4)
  6. customThe solvent was evaporated at room temperature under vacuum
  7. customThe resulting crude material was purified by silica gel chromatography (eluting with 50% EtOAc in Hexane)

出典と根拠

ORDレコード
ord-b7f0698470c24fe8819065848a90b29b
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08551914B2

反応ノート

読み込み中…

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