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Potassium Carbonate → 4-Methoxy-3-(3-morpholinopropoxy)benzonitrile

HRID 715683
ノート
印刷プレビュー

反応式

HRID 715683 の反応式
[N:1]1([CH2:7][CH2:8][CH2:9][OH:10])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.CS(Cl)(=O)=O.C(=O)([O-])[O-].[K+].[K+].O[C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][C:30]=1[O:31][CH3:32])[C:26]#[N:27]>ClCCl>[CH3:32][O:31][C:30]1[CH:29]=[CH:28][C:25]([C:26]#[N:27])=[CH:24][C:23]=1[O:10][CH2:9][CH2:8][CH2:7][N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 1995763-Morpholino-1-propanolHCID 49128223-Hydroxy-4-methoxybenzonitrile

生成物 1

HCID 103560884-Methoxy-3-(3-morpholinopropoxy)benzonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

5 g 3-Morpholine-4-yl-propan-1-ol was dissolved in dichloromethane, cooled to 0° C., 3.25 mL methanesulfonylchloride was added and the mixture was stirred for 2 h at ambient temperature. Then 7 g potassium carbonate and 3-hydroxy-4-methoxybenzonitrile were added and the reaction was stirred at 45° C. for 3 h. The mixture was concentrated and 70 mL dimethylacetamide was added and stirred at 120° C. for 3 h. After this time, the mixture was diluted with dichloromethane and extracted with water, the organic phase was dried over magnesium sulfate and concentrated.

後処理

  1. stirringthe reaction was stirred at 45° C. for 3 h
  2. concentrationThe mixture was concentrated
  3. addition70 mL dimethylacetamide was added
  4. stirringstirred at 120° C. for 3 h
  5. additionAfter this time, the mixture was diluted with dichloromethane
  6. extractionextracted with water
  7. dry with materialthe organic phase was dried over magnesium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-7af5c63f4222416bbf2ffc0f49886eaf
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187478B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート