Potassium Carbonate → Buspirone

HRID 1649476

반응식

HRID 1649476 반응식
[CH2:1]1[CH2:5][C:4]2([CH2:12][C:10](=[O:11])[NH:9][C:7](=[O:8])[CH2:6]2)[CH2:3][CH2:2]1.[Br-].[N:14]1[CH:19]=[CH:18][CH:17]=[N:16][C:15]=1[N:20]1[CH2:29][CH2:28][N+:23]2([CH2:27][CH2:26][CH2:25][CH2:24]2)[CH2:22][CH2:21]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N:14]1[CH:19]=[CH:18][CH:17]=[N:16][C:15]=1[N:20]1[CH2:29][CH2:28][N:23]([CH2:24][CH2:25][CH2:26][CH2:27][N:9]2[C:7](=[O:8])[CH2:6][C:4]3([CH2:5][CH2:1][CH2:2][CH2:3]3)[CH2:12][C:10]2=[O:11])[CH2:22][CH2:21]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1368438-Azaspiro(4.5)decane-7,9-dioneHCID 6575058-Aza-5-azoniaspiro(4.5)decane, 8-(2-pyrimidinyl)-, bromide (1:1)

생성물 1

HCID 2477Buspirone

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture 3,3-tetramethyleneglutarimide (16.7 g., 0.1 mole), 8-(2-pyrimidinyl)-8-aza-5-azoniaspiro[4.5]decane bromide (29.9 g., 0.1 mole) and potassium carbonate (16.6 g., 0.12 mole) in 190 ml. of dimethylformamide is maintained at 150°-155° C. for a reaction period of 24 hours and then evaporated to dryness under reduced pressure. The resulting solid is triturated with 90 ml. of water, taken up in 10% hydrochloric acid and filtered. The acid filtrate is made basic with 10% aqueous sodium hydroxide and precipitated free base collected and dried to provide 8-[4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl]-8-azaspiro[4.5]decane-7,9-dione.

후처리

  1. customevaporated to dryness under reduced pressure
  2. customThe resulting solid is triturated with 90 ml
  3. filtrationfiltered
  4. customprecipitated free base
  5. customcollected
  6. customdried

출처 및 근거

ORD 기록
ord-5fb23b2414a048f0b782e42ec82c51d3
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04417049

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