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Potassium Carbonate → HCID 53311788、化合物

HRID 1401759
ノート
印刷プレビュー

反応式

HRID 1401759 の反応式
[CH3:1][C:2]1([CH3:25])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14]3[N:15]=[C:16]([N:19]4[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]4)[S:17][CH:18]=3)[CH:5]=[CH:4][C:3]1=2.C([O:29][CH2:30][CH2:31][CH2:32][CH2:33]Br)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.ClCCl>[CH3:1][C:2]1([CH3:25])[CH2:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:8]2[CH:7]=[C:6]([C:14]3[N:15]=[C:16]([N:19]4[CH2:20][CH2:21][N:22]([CH2:33][CH2:32][CH2:31][CH2:30][OH:29])[CH2:23][CH2:24]4)[S:17][CH:18]=3)[CH:5]=[CH:4][C:3]1=2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 784911-Butanol, 4-bromo-, 1-acetateHCID 53312286HCID 53312286、化合物

生成物 1

HCID 53311788HCID 53311788、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
60 °C

実験手順

120 mg (0.34 mmol) of 1-[4-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)thiazol-2-yl]piperazine were suspended in 3 ml of DMF with 100 μl (0.68 mmol) of 4-bromobutyl acetate and 56 mg (0.41 mmol) of potassium carbonate and stirred at 60° C. overnight. The reaction mixture was taken up in dichloromethane, washed once each with a concentrated sodium hydrogencarbonate solution and a 1N hydrochloric acid solution. The organic phase was dried over sodium sulfate, filtered and evaporated. The protecting group is cleaved off by means of a 1N NaOH solution in methanol: The reaction mixture was stirred at room temperature and subsequently evaporated. The product was purified by means of preparative HPLC and converted into the hydrochloride by treatment with methanolic HCl.

後処理

  1. washwashed once each with a concentrated sodium hydrogencarbonate solution
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. stirringThe reaction mixture was stirred at room temperature
  6. customsubsequently evaporated
  7. customThe product was purified by means of preparative HPLC

出典と根拠

ORDレコード
ord-31555aa9aa8a4cca9c917947d45d61a8
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08907098B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート