N-Methylcyclohexylamine → 4-[[(N-cyclohexyl-N-methylamino)methylene]amino]-3-pyridinol

HRID 361329

반응식

HRID 361329 반응식
[CH3:1][N:2]([CH:4]=[N:5][C:6]1[CH:11]=[CH:10][N:9]=[CH:8][C:7]=1[OH:12])[CH3:3].CN[CH:15]1[CH2:20][CH2:19]C[CH2:17][CH2:16]1>C1(C)C=CC=CC=1>[CH:3]1([N:2]([CH:4]=[N:5][C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[OH:12])[CH3:1])[CH2:19][CH2:20][CH2:15][CH2:16][CH2:17]1

참가 물질

4

반응물 2

HCID 7514N-MethylcyclohexylamineHCID 153809294-[[(Dimethylamino)methylene]amino]-3-pyridinol

생성물 1

HCID 153809374-[[(N-cyclohexyl-N-methylamino)methylene]amino]-3-pyridinol수율 83.8%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 4-[[(dimethylamino)methylene]amino]-3-pyridinol (5.00 g), N-methylcyclohexylamine (5.20 g), and anhydrous toluene (50 mL) was heated at reflux under nitrogen for 17 hours. The solution was concentrated under reduced pressure and the crude product chromatographed on silica gel (10% methanol in dichloromethane) to afford 5.92 g of solid. Recrystallization from ethyl acetate/hexanes afforded 4.90 g of crystalline material, m.p. 127°-129° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux under nitrogen for 17 hours
  3. concentrationThe solution was concentrated under reduced pressure
  4. customthe crude product chromatographed on silica gel (10% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-73fb4cacfe7142d4ba70dc2957007909
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866565

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