Hydrochloric Acid → 4,4-Dimethyl-1-(4-(4-(4-(1,1-dimethylethyl)-2-thiazolyl)-1-piperazinyl)butyl)-2,6-piperidin-dione

HRID 329606

반응식

HRID 329606 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:11](=[O:12])[CH2:10][C:9]([CH3:14])([CH3:13])[CH2:8][C:7]1=[O:15].[CH3:16][C:17]([C:20]1[N:21]=[C:22]([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[S:23][CH:24]=1)([CH3:19])[CH3:18].C([O-])([O-])=O.[K+].[K+].Cl>O.C(O)C.CCOCC.CN(C)C=O>[CH3:13][C:9]1([CH3:14])[CH2:10][C:11](=[O:12])[N:6]([CH2:5][CH2:4][CH2:3][CH2:2][N:28]2[CH2:29][CH2:30][N:25]([C:22]3[S:23][CH:24]=[C:20]([C:17]([CH3:19])([CH3:18])[CH3:16])[N:21]=3)[CH2:26][CH2:27]2)[C:7](=[O:15])[CH2:8]1

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 136603351-(4-Bromobutyl)-4,4-dimethylpiperidine-2,6-dioneHCID 198712791-(4-(1,1-Dimethylethyl)-2-thiazolyl)-piperazine

생성물 1

HCID 137477334,4-Dimethyl-1-(4-(4-(4-(1,1-dimethylethyl)-2-thiazolyl)-1-piperazinyl)butyl)-2,6-piperidin-dione

시약·촉매·용매 3

HCID 962Water용매2회HCID 6228Dimethylformamide용매HCID 21585056Diethyl ether ethanol용매

실험 절차

4 g 1-(4-Bromobutyl)-4,4-dimethyl-2,6-piperidin-dione, 3.15 g 1-(4-(1,1-dimethylethyl)-2-thiazolyl)-piperazine, 2.7 g K2CO3, 70 ml dimethylformamide and 20 ml water are stirred at room temperature for about 35 hours. The mixture is diluted with water, extracted twice with ether, the combined extracts are washed with water, dried (Na2SO4) and evaporated. The residue is recrystallized from hexane/ethyl acetate, whereby the title compound is obtained, m.p. 93°-94°. M.p. of the hydrochloride is 199°-201° (ethanol/ether).

후처리

  1. extractionextracted twice with ether
  2. washthe combined extracts are washed with water
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe residue is recrystallized from hexane/ethyl acetate, whereby the title compound
  6. customis obtained
  7. customis 199°-201°

출처 및 근거

ORD 기록
ord-5f01b3268e334e29afc05a72f5dd0b2e
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892879

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