Acetic Anhydride → HCID 19828478、化合物

HRID 1494525ノート

反応式

HRID 1494525 の反応式
[CH3:1][C:2]1([CH3:22])[O:7][CH2:6][C:5]2[C:8]([CH:13]([OH:21])[C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=3)=[CH:9][N:10]=[C:11]([CH3:12])[C:4]=2[O:3]1.[C:23](OC(=O)C)(=[O:25])[CH3:24].C([O-])(O)=O.[Na+]>N1C=CC=CC=1>[CH3:1][C:2]1([CH3:22])[O:7][CH2:6][C:5]2[C:8]([CH:13]([O:21][C:23](=[O:25])[CH3:24])[C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=3)=[CH:9][N:10]=[C:11]([CH3:12])[C:4]=2[O:3]1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 11529834(4-chlorophenyl)-(2,2,8-trimethyl-4H-[1,3]dioxino[4,5-c]pyridin-5-yl)methanol

生成物 1

HCID 19828478HCID 19828478、化合物収率 100%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

210 mg (0.66 mmoles) of (+)-2,2,8-trimethyl-5-(4-chloro-α-hydroxybenzyl)-pyrido-[4,3-e]-1,3-dioxane are poured into a 2 ml vial and dissolved in 500 μl of pyridine and 110 μl of acetic anhydride (1.16 mmole). The reaction mixture is stirred for 18 hours, then poured into 30 ml of saturated NaHCO3. The mixture is allowed to stir at room temperature for 1 hour, then extracted with 3×30 ml of CH2Cl2. The combined CH2Cl2 layers are washed with 3×20 ml of 2N HCl. The organic phase is dried over Na2SO4, filtered and the filtrate is evaporated to dryness. 24 g are obtained as a white solid with a yield of 100%.

後処理

  1. stirringto stir at room temperature for 1 hour
  2. extractionextracted with 3×30 ml of CH2Cl2
  3. washThe combined CH2Cl2 layers are washed with 3×20 ml of 2N HCl
  4. dry with materialThe organic phase is dried over Na2SO4
  5. filtrationfiltered
  6. customthe filtrate is evaporated to dryness
  7. custom24 g are obtained as a white solid with a yield of 100%

出典と根拠

ORDレコード
ord-b873f21db5254fceb310d1cb3d3da07a
出典データセット
uspto-grants-1991_06
特許番号
US05026855

反応ノート

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