Morpholine → 4-(2-Hydrazinyl-6-methyl-4-pyrimidinyl)morpholine

HRID 2074976ノート

反応式

HRID 2074976 の反応式
Cl[C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([CH3:9])[N:3]=1.[NH:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1.O.[NH2:17][NH2:18]>CO>[NH:17]([C:2]1[N:7]=[C:6]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[CH:5]=[C:4]([CH3:9])[N:3]=1)[NH2:18]

参加物

5

反応物 3

HCID 8083MorpholineHCID 24654Hydrazine hydrate (1:1)HCID 794712,4-Dichloro-6-methylpyrimidine

生成物 1

HCID 668584764-(2-Hydrazinyl-6-methyl-4-pyrimidinyl)morpholine収率 59.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 2,4-dichloro-6-methylpyrimidine (0.41 g, 2.50 mmol) in MeOH (5 mL) was added morpholine (0.5 mL, 5.73 mmol). The solution was stirred for 30 min at room temperature, and then hydrazine monohydrate (1.0 mL, 20.6 mmol) was added. The solution was then heated at 60° C. and stirred for 16 h. The solution was then cooled to room temperature and purified by reverse phase HPLC to afford 0.31 g of the title compound (59%) as a waxy white solid. MH+210.

後処理

  1. temperatureThe solution was then heated at 60° C.
  2. stirringstirred for 16 h
  3. temperatureThe solution was then cooled to room temperature
  4. custompurified by reverse phase HPLC

出典と根拠

ORDレコード
ord-da1608fe464742fc891b2316e834ad4b
出典データセット
uspto-grants-2011_04
特許番号
US07919528B2

反応ノート

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