Hydrochloric Acid → Eslicarbazepine Acetate

HRID 526679노트

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HRID 526679 반응식
[CH:1]1[CH:2]=[CH:3][C:4]2[N:15]([C:16]([NH2:18])=[O:17])[C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[C@@H:8]([OH:19])[CH2:7][C:5]=2[CH:6]=1.CN(C1C=CC=CN=1)C.[C:29](OC(=O)C)(=[O:31])[CH3:30].Cl>O.ClCCl.C(N(CC)CC)C>[CH3:30][C:29]([O:19][C@@H:8]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=2[N:15]([C:16]([NH2:18])=[O:17])[C:4]2[CH:3]=[CH:2][CH:1]=[CH:6][C:5]=2[CH2:7]1)=[O:31]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 218852-DimethylaminopyridineHCID 9881504Eslicarbazepine

생성물 1

HCID 179344Eslicarbazepine Acetate

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

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온도
22.5 °C

실험 절차

To a solution of eslicarbazepine (30 gm), triethylamine (19.7 gm), dimethylaminopyridine (0.15 gm), and dichloromethane (150 mL), acetic anhydride (14.5 mL in 14.5 mL dichloromethane) was added and solution was stirred at about 20-25° C. for about 3 hrs. The resulting solution was cooled to about 10-15° C. To the resulting solution water (90 mL) was added followed by addition of HCl till pH of the resulting solution was 1-2. Organic layer was separated and washed with water. Water was added to organic layer followed by cooling to about 10-15° C. The pH of the resulting solution was adjusted to 9-10 by adding NaOH (10% w/v) solution. Organic layer was separated and solvent was distilled out completely to obtain the title compound.

후처리

  1. temperatureThe resulting solution was cooled to about 10-15° C
  2. customOrganic layer was separated
  3. washwashed with water
  4. additionWater was added to organic layer
  5. temperatureby cooling to about 10-15° C
  6. additionby adding NaOH (10% w/v) solution
  7. customOrganic layer was separated
  8. distillationsolvent was distilled out completely

출처 및 근거

ORD 기록
ord-f5b8673a21564b17a1acbf6fdb988e98
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346760B2

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