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Hydrochloric Acid → (S)-1-Isopropyl-3-methyl-piperazine

HRID 879604
ノート
印刷プレビュー

反応式

HRID 879604 の反応式
C([N:8]1[CH2:13][CH2:12][N:11]([CH:14]([CH3:16])[CH3:15])[CH2:10][C@@H:9]1[CH3:17])(OC(C)(C)C)=O.Cl>O1CCOCC1>[CH:14]([N:11]1[CH2:12][CH2:13][NH:8][C@@H:9]([CH3:17])[CH2:10]1)([CH3:16])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86700418(S)-1-Boc-2-methyl-4-isopropylpiperazine

生成物 1

HCID 59771337(S)-1-Isopropyl-3-methyl-piperazine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To crude (S)-1-Boc-2-methyl-4-isopropylpiperazine in 1,4-dioxane (10 mL) was added HCl (5 mL of a 4M solution in 1,4-dioxane). The reaction mixture was stirred at room temperature for 28 h then concentrated. The resulting solid was suspended in diethyl ether, concentrated and dried on high vacuum for 1 d. The resulting solid was taken up in aq. 2N NaOH and the solution extracted three times with DCM. The combined organic layers were dried over sodium sulfate, filtered, and concentrated to provide the free base of the product which was used without further purification. LCMS-ESI+: calc'd for C8H18N2 (M+H+): 143.1; Found: 143.7 (M+H+).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. concentrationthen concentrated
  2. concentrationconcentrated
  3. customdried on high vacuum for 1 d
  4. extractionthe solution extracted three times with DCM
  5. dry with materialThe combined organic layers were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto provide the free base of the product which
  9. customwas used without further purification

出典と根拠

ORDレコード
ord-b5dff1e3c1c84c3dafeedd4b6241aae5
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987250B2

反応ノート

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