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Hydrochloric Acid → 4-[N-methyl-N-(3-cyclopropylmethylamino-2-pyridinyl) amino]piperidine

HRID 361835
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반응식

HRID 361835 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH3:26])[C:15]2[C:20]([NH:21][CH2:22][CH:23]3[CH2:25][CH2:24]3)=[CH:19][CH:18]=[CH:17][N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>O1CCOCC1>[CH3:26][N:14]([CH:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1)[C:15]1[C:20]([NH:21][CH2:22][CH:23]2[CH2:24][CH2:25]2)=[CH:19][CH:18]=[CH:17][N:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 107610091-tert-Butyloxycarbonyl-4-[N-methyl-N-(3-cyclopropylmethylamino-2-pyridinyl)amino]piperidine

생성물 1

HCID 107538574-[N-methyl-N-(3-cyclopropylmethylamino-2-pyridinyl) amino]piperidine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1-tert-Butyloxycarbonyl-4-[N-methyl-N-(cyclopropylmethylamino-2-pyridinyl)amino]piperidine (EXAMPLE 161, 1.46 g, 4.05 mmol) is dissolved in 10 ml dioxane. Hydrochloric acid (30 ml of 4.0M in dioxane) is added. The solvent is removed by evaporation and the residue is suspended in water. The water is adjusted to pH=12 with sodium hydroxide (1N) and extracted with chloroform/methanol. The organic phase is dried over sodium sulfate and the solvent evaporated to give the title compound, NMR (300 MHz, CD3OD) 7.37, 6.77, 3.3-3.5, 2.85, 2.79, 2.45, 2.36, 1.53, 1.40, 0.92, 0.33 and 0.56δ.

후처리

  1. customThe solvent is removed by evaporation
  2. extractionextracted with chloroform/methanol
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-1416b9f47f9d4686a0d61019b7536ee7
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05866589

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