2-(Isopropylamino)ethanol → 2-[N-Isopropyl-N-(2-benzoxazolyl)amino]ethanol

HRID 257181ノート

反応式

HRID 257181 の反応式
Cl[C:2]1[O:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[CH:11]([NH:14][CH2:15][CH2:16][OH:17])([CH3:13])[CH3:12].C(N(CC)CC)C>O1CCCC1>[CH:11]([N:14]([CH2:15][CH2:16][OH:17])[C:2]1[O:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1)([CH3:13])[CH3:12]

参加物

5

反応物 3

HCID 79942-(Isopropylamino)ethanolHCID 8471TriethylamineHCID 119862-Chlorobenzoxazole

生成物 1

HCID 101048742-[N-Isopropyl-N-(2-benzoxazolyl)amino]ethanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2-Chlorobenzoxazole (23.04 g) was added dropwise to an ice-cooled solution of 2-(isopropylamino)ethanol (15.45 g) and triethylamine (30.3 g) in tetrahydrofuran (500 ml). The mixture was stirred at room temperature for 30 minutes, then heated at reflux overnight before being cooled and evaporated. The residue was dissolved in dichloromethane (800 ml) and washed with saturated sodium bicarbonate solution (500 ml), water (3×11) brine (11), dried (MgSO4), filtered and evaporated. The title compound was obtained as an oil following chromatography on silica gel using 1.5% methanol-dichloromethane as solvent.

後処理

  1. temperatureheated
  2. temperatureat reflux overnight
  3. temperaturebefore being cooled
  4. customevaporated
  5. dissolutionThe residue was dissolved in dichloromethane (800 ml)
  6. washwashed with saturated sodium bicarbonate solution (500 ml), water (3×11) brine (11)
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. customevaporated

出典と根拠

ORDレコード
ord-bbb0b4fbebbc44c082dcf195a17cbd07
出典データセット
uspto-grants-1993_11
特許番号
US05260445

反応ノート

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