Hydrochloric Acid → (S)-2-Isopropylpiperazine

HRID 1911426ノート

反応式

HRID 1911426 の反応式
[CH3:1][CH:2]([C@H:4]1[CH2:9][NH:8][CH2:7][CH2:6][N:5]1C(OC(C)(C)C)=O)[CH3:3].Cl>C(OCC)(=O)C.CO.O1CCOCC1>[CH3:1][CH:2]([C@H:4]1[CH2:9][NH:8][CH2:7][CH2:6][NH:5]1)[CH3:3]

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 17750439(2S)-2-Isopropylpiperazine, N1-BOC protected

生成物 1

HCID 15023839(S)-2-Isopropylpiperazine収率 94%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of tert-butyl (2S)-2-propan-2-ylpiperazine-1-carboxylate (2 g, 8.76 mmol) in a mixture of ethyl acetate (20 mL) and methanol (20.00 mL) was stirred at room temperature with 4M HCl in dioxane (30 mL) for 40 h under nitrogen. The reaction mixture was evaporated to dryness. The crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 3.5M NH3/MeOH and pure fractions were evaporated to dryness to afford (2S)-2-propan-2-ylpiperazine (1.052 g, 94%) as a white solid.

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. customThe crude product was purified by ion exchange chromatography
  3. washThe desired product was eluted from the column
  4. customwere evaporated to dryness

出典と根拠

ORDレコード
ord-a85d2b8847ec4486bfcf60e252d5abf4
出典データセット
uspto-grants-2013_12
特許番号
US08604022B2

反応ノート

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