6-Nitroveratraldehyde → 6-Nitroveratrylidene-2-aminomethyltetrahydropyran

HRID 436452ノート

反応式

HRID 436452 の反応式
[NH2:1][CH2:2][CH:3]1[CH2:8][CH2:7][CH2:6][CH2:5][O:4]1.[N+:9]([C:12]1[C:17]([CH:18]=O)=[CH:16][C:15]([O:20][CH3:21])=[C:14]([O:22][CH3:23])[CH:13]=1)([O-:11])=[O:10]>C(O)C>[N+:9]([C:12]1[C:17]([CH:18]=[C:8]2[CH2:7][CH2:6][CH2:5][O:4][CH:3]2[CH2:2][NH2:1])=[CH:16][C:15]([O:20][CH3:21])=[C:14]([O:22][CH3:23])[CH:13]=1)([O-:11])=[O:10]

参加物

4

反応物 2

HCID 885056-NitroveratraldehydeHCID 97924(Tetrahydro-2H-pyran-2-ylmethyl)amine

生成物 1

HCID 542260806-Nitroveratrylidene-2-aminomethyltetrahydropyran

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of 2-aminomethyltetrahydropyran (51 g, 0.44 mole) and ethanol (50 ml) was slowly added to a heated suspension of 6-nitroveratraldehyde (84 g, 0.4 mole) and ethanol (600 ml). The resulting solution was refluxed for 1.5 hrs and cooled overnight. The solution was concentrated to dryness and the oil was disolved in chloroform and washed with water. The chloroform extract was concentrated leaving a dark oil which crystallized upon standing. The solid was suspended in hexane and filtered (117 g. 95%), m.p. 89°-96°.

後処理

  1. temperatureThe resulting solution was refluxed for 1.5 hrs
  2. temperaturecooled overnight
  3. concentrationThe solution was concentrated to dryness
  4. washwashed with water
  5. extractionThe chloroform extract
  6. concentrationwas concentrated
  7. customleaving a dark oil which
  8. customcrystallized
  9. filtrationfiltered (117 g. 95%), m.p. 89°-96°

出典と根拠

ORDレコード
ord-6a848c78ed574a8b88d1cdd5376757d9
出典データセット
uspto-grants-1977_02
特許番号
US04009177

反応ノート

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