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

HRID 329606

反応式

HRID 329606 の反応式
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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒HCID 21585056Diethyl ether ethanol溶媒

実験手順

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).

後処理

  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°

出典と根拠

ORDレコード
ord-5f01b3268e334e29afc05a72f5dd0b2e
出典データセット
uspto-grants-1990_01
特許番号
US04892879

関連ノート

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