Acetic Anhydride → HCID 19828478, 화합물

HRID 1494525노트

반응식

HRID 1494525 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 19828478HCID 19828478, 화합물수율 100%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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%.

후처리

  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%

출처 및 근거

ORD 기록
ord-b873f21db5254fceb310d1cb3d3da07a
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05026855

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