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

HRID 879604
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HRID 879604 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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+).

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후처리

  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

출처 및 근거

ORD 기록
ord-b5dff1e3c1c84c3dafeedd4b6241aae5
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987250B2

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