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

HRID 362196

反応式

HRID 362196 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-37c99f83914c4ca58690a7333dfd8aca
出典データセット
uspto-grants-1999_02
特許番号
US05869480

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