Hydrochloric Acid → Eslicarbazepine Acetate

HRID 526679ノート

反応式

HRID 526679 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 179344Eslicarbazepine Acetate

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒

反応条件

温度
22.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f5b8673a21564b17a1acbf6fdb988e98
出典データセット
uspto-grants-2016_05
特許番号
US09346760B2

反応ノート

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