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Ethanolamine → HCID 178429079、化合物

HRID 1869003
ノート
印刷プレビュー

反応式

HRID 1869003 の反応式
C([O:4][C@@H:5]1[C@@H:10]([O:11]C(=O)C)[C@H:9]([O:15]C(=O)C)[C@@H:8]([CH2:19][O:20]C(=O)C)[O:7][C@H:6]1[O:24][C:25]1[C:29]([CH2:30][C:31]2[CH:36]=[CH:35][C:34](OCCN)=[CH:33][C:32]=2[CH3:41])=[C:28]([CH:42]([CH3:44])[CH3:43])[NH:27][N:26]=1)(=O)C.[CH3:45][S:46]([N:49]=[C:50](OC1C=CC=CC=1)OC1C=CC=CC=1)(=[O:48])=[O:47].[NH2:65][CH2:66][CH2:67][OH:68]>O1CCCC1>[C@@H:6]1([O:24][C:25]2[C:29]([CH2:30][C:31]3[CH:36]=[CH:35][C:34]([O:68][CH2:67][CH2:66][NH:65][C:50]([NH:65][CH2:66][CH2:67][OH:68])=[N:49][S:46]([CH3:45])(=[O:47])=[O:48])=[CH:33][C:32]=3[CH3:41])=[C:28]([CH:42]([CH3:43])[CH3:44])[NH:27][N:26]=2)[O:7][C@H:8]([CH2:19][OH:20])[C@@H:9]([OH:15])[C@H:10]([OH:11])[C@H:5]1[OH:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 700EthanolamineHCID 13738851N-(Diphenoxymethylene)-methanesulfonamideHCID 689452653-(2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyloxy)-4-{[4-(2-aminoethoxy)-2-methylphenyl]methyl}-5-isopropyl-1H-pyrazole

生成物 1

HCID 178429079HCID 178429079、化合物収率 76.5%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of dichlorophenoxymethane (1 g) in acetonitrile (10 mL) was added methanesulfonamide (0.39 g) under ice-cooling, and the mixture was stirred at room temperature for 48 hours. The reaction mixture was poured into a saturated aqueous sodium hydrogen carbonate solution, and the resuling mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give 1-(N-methanesulfonylimino)-1,1-diphenoxymethane (0.95 g). To a solution of 3-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyloxy)-4-{[4-(2-aminoethoxy)-2-methylphenyl]methyl}-5-isopropyl-1H-pyrazole (50 mg) in tetrahydrofuran (1 mL) was added 1-(N-methanesulfonylimino)-1,1-diphenoxymethane (26 mg) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. To the reaction mixture was added 2-aminoethanol (49 mg), and the mixture was stirred at 60° C. overnight. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in methanol (2 mL). To the solution was added sodium methoxide (28% methanol solution, 0.008 mL), and the mixture was stirred at room temperature for 3 hours. To the reaction mixture was added acetic acid (0.01 mL). The resulting mixture was concentrated under reduced pressure, and the residue was purified by solid phase extraction on ODS (washing solvent: distilled water, eluent: methanol) to give the title compound (38 mg).

後処理

  1. temperaturecooling
  2. stirringthe mixture was stirred at 60° C. overnight
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in methanol (2 mL)
  5. additionTo the solution was added sodium methoxide (28% methanol solution, 0.008 mL)
  6. stirringthe mixture was stirred at room temperature for 3 hours
  7. additionTo the reaction mixture was added acetic acid (0.01 mL)
  8. concentrationThe resulting mixture was concentrated under reduced pressure
  9. distillationthe residue was purified by solid phase extraction on ODS (washing solvent: distilled water, eluent: methanol)

出典と根拠

ORDレコード
ord-0c57ba28cf6a455ca5ed356f3bd8c59b
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07635684B2

反応ノート

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