Hydrochloric Acid → HCID 67113455、化合物

HRID 2088898ノート

反応式

HRID 2088898 の反応式
C(O)(=O)CCC(O)=O.[F:9][C:10]([F:37])([F:36])[C:11]1[N:12]=[C:13]([CH:23]2[CH2:28][CH2:27][N:26](C(OC(C)(C)C)=O)[CH2:25][CH2:24]2)[N:14]([CH2:16][CH2:17][N:18]2[CH2:22][CH2:21][CH2:20][CH2:19]2)[CH:15]=1.Cl>CO>[F:37][C:10]([F:9])([F:36])[C:11]1[N:12]=[C:13]([CH:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[N:14]([CH2:16][CH2:17][N:18]2[CH2:22][CH2:21][CH2:20][CH2:19]2)[CH:15]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67954408tert-Butyl 4-(4-(trifluoromethyl)-1-(2-pyrrolidin-1-ylethyl)-1H-imidazol-2-yl)piperidine-1-carboxylate succinate

生成物 1

HCID 67113455HCID 67113455、化合物収率 96%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

Add tert-butyl 4-(4-(trifluoromethyl)-1-(2-pyrrolidin-1-ylethyl)-1H-imidazol-2-yl)piperidine-1-carboxylate succinate (120 g, 224.48 mmol) in methanol (720 mL) to 37% aqueous hydrogen chloride (76.08 mL, 4 eq) at room temperature. Stir the solution at 50° C. Concentrate the reaction mixture. Add 500 mL water and wash with methyl tert-butyl ether (200 mL). Basify the aqueous solution with 6M aqueous sodium hydroxide at 0° C. Extract with ethyl acetate (4×200 mL). Dry the organics over anhydrous sodium sulfate and concentrate in vacuo to give the title compound (68 g, 96%). MS (ES) m/z=317 [M]+.

後処理

  1. concentrationConcentrate the reaction mixture
  2. additionAdd 500 mL water
  3. washwash with methyl tert-butyl ether (200 mL)
  4. customat 0° C
  5. extractionExtract with ethyl acetate (4×200 mL)
  6. dry with materialDry the organics over anhydrous sodium sulfate
  7. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-b6fd0cc4aabe46ff9bc7fa299a2755f4
出典データセット
uspto-grants-2013_05
特許番号
US08436002B2

反応ノート

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