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2,4,6-Trimethylpyridine → 2-octadecyl-7-(2,3,4,6-tetra-O-acetyl beta-D-galactopyranosyloxy)-3H-phenoxazin-3-one

HRID 4880
ノート
印刷プレビュー

反応式

HRID 4880 の反応式
[OH:1][C:2]1[CH:3]=[C:4]2[C:13](=[CH:14][CH:15]=1)[N:12]=[C:11]1[C:6](=[CH:7][C:8](=[O:34])[C:9]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])=[CH:10]1)[O:5]2.CC1C=C(C)N=C(C)C=1.[CH3:44][C:45]([O:47][CH2:48][CH:49]1[O:54][C@H:53](Br)[CH:52]([O:56][C:57]([CH3:59])=[O:58])[C@@H:51]([O:60][C:61]([CH3:63])=[O:62])[C@H:50]1[O:64][C:65]([CH3:67])=[O:66])=[O:46]>ClCCl.C(=O)([O-])[O-].[Ag+2]>[CH2:16]([C:9]1[C:8](=[O:34])[CH:7]=[C:6]2[C:11](=[N:12][C:13]3[C:4]([O:5]2)=[CH:3][C:2]([O:1][C@@H:53]2[O:54][C@H:49]([CH2:48][O:47][C:45](=[O:46])[CH3:44])[C@H:50]([O:64][C:65](=[O:66])[CH3:67])[C@H:51]([O:60][C:61](=[O:62])[CH3:63])[C@H:52]2[O:56][C:57](=[O:58])[CH3:59])=[CH:15][CH:14]=3)[CH:10]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]
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 3

HCID 79532,4,6-TrimethylpyridineHCID 24802013Acetobromo-a-D-galactoseHCID 178418639HCID 178418639、化合物

生成物 1

HCID 228467472-octadecyl-7-(2,3,4,6-tetra-O-acetyl beta-D-galactopyranosyloxy)-3H-phenoxazin-3-one

試薬・触媒・溶媒 2

HCID 178418647HCID 178418647、化合物触媒
HCID 6344
Dichloromethane
溶媒

実験手順

A mixture of 7-hydroxy-2-octadecyl-3H-phenoxazine-3-one ("octadecylresorufin) (220 mg, 0.47 mmole), powdered, activated 4Å molecular sieves (0.5 g), sym-collidine (125 μL, 0.95 mmole), and silver carbonate (155 mg, 0.56 mmole) in dry dichloromethane (20 mL) is allowed to stir at room temperature, under an atmosphere of dry nitrogen gas, in the dark for 1 hour. To this mixture is added 1-bromo-2,3,4,6-tetra-O-acetyl-α-D-galactopyranoside (389 mg, 0.95 mmole), slowly with stirring, and the resulting heterogenous solution allowed to stir as above for 72 hours. After this time the reaction mixture is filtered through a pad of diatomaceous earth. The precipitate is washed with chloroform (5×10 mL) and the combined organic filtrates are extracted with 1M aqueous HCl (1×75 mL), saturated aqueous sodium bicarbonate solution (1×75 mL), 1M sodium thiosulfate (1×75 mL), and water (1×75 mL). The organic layer is dried over anhydrous sodium sulfate, filtered, evaporated under reduced pressure, and dried in vacuo to an orange-brown powder (440 mg). An analytical sample of the title compound can be isolated by preparative t.l.c. (20×20 cm SiO2 plate; eluent=9:1 chloroform:ethylacetate) with the bright-orange product eluting at the highest Rf (0.44), (50 mg from 200 mg applied).

後処理

  1. stirringslowly with stirring
  2. stirringto stir as above for 72 hours
  3. filtrationAfter this time the reaction mixture is filtered through a pad of diatomaceous earth
  4. washThe precipitate is washed with chloroform (5×10 mL)
  5. extractionthe combined organic filtrates are extracted with 1M aqueous HCl (1×75 mL), saturated aqueous sodium bicarbonate solution (1×75 mL), 1M sodium thiosulfate (1×75 mL), and water (1×75 mL)
  6. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. customevaporated under reduced pressure
  9. dry with materialdried in vacuo to an orange-brown powder (440 mg)

出典と根拠

ORDレコード
ord-524d531152204c2e8e6ceed8643f94a1
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05242805

反応ノート

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