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Hydrochloric Acid → 1-(4-chlorophenyl)-N3,N3-dimethylpropane-1,3-diamine

HRID 423052
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인쇄 미리보기

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HRID 423052 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([NH:15]C(=O)OC(C)(C)C)[CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])=[CH:5][CH:4]=1>C(Cl)Cl.CO>[Cl:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]([NH2:15])[CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])=[CH:7][CH:8]=1
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 57750395HCID 57750395, 화합물2회

생성물 1

HCID 115575541-(4-chlorophenyl)-N3,N3-dimethylpropane-1,3-diamine수율 94%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

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온도
22 °C

실험 절차

Hydrogen chloride (4M in dioxane, 1.132 mL, 32.61 mmol) was added to tert-butyl 1-(4-chlorophenyl)-3-(dimethylamino)propylcarbamate (Intermediate 32) (0.051 g, 0.16 mmol) in a mixture of DCM (5 mL) and methanol (2 mL) at 22° C. The resulting solution was stirred at 22° C. for 4 hours. The mixture was concentrated and the residue was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 2M NH3/MeOH and pure fractions were evaporated to dryness to afford 1-(4-chlorophenyl)-N3,N3-dimethylpropane-1,3-diamine (0.032 g, 92%) as a colourless oil.

후처리

  1. concentrationThe mixture was concentrated
  2. customthe residue was purified by ion exchange chromatography
  3. washThe desired product was eluted from the column
  4. customwere evaporated to dryness

출처 및 근거

ORD 기록
ord-3ecd8b09d8204254af985f87f24b941d
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101623B2

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