4-Methylmorpholine → HCID 68802054、化合物

HRID 924625

反応式

HRID 924625 の反応式
[CH2:1]([O:3][C:4](=[O:11])[C:5]([CH3:10])([CH3:9])[C:6]([OH:8])=O)[CH3:2].[NH2:12][CH2:13][CH2:14][N:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1.CN1CCOCC1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F>O1CCCC1>[CH2:1]([O:3][C:4](=[O:11])[C:5]([CH3:10])([CH3:9])[C:6]([NH:12][CH2:13][CH2:14][N:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1)=[O:8])[CH3:2]

参加物

6

反応物 4

HCID 79724-MethylmorpholineHCID 2317543-Ethoxy-2,2-dimethyl-3-oxopropanoic acidHCID 4082852-MorpholinoethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate

生成物 1

HCID 68802054HCID 68802054、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
5 °C

実験手順

19 g 2,2-Dimethyl-malonic acid monoethyl ester were weighed into a round-bottomed flask and under N2 atmosphere and room temperature, 200 ml tetrahydrofurane, 15.6 ml 4-(2-Aminoethyl)-morpholine and 32.6 ml N-Methylmorpholine were added. The reaction was stirred and cooled down to 5° C. Then, 43.8 g TBTU were added and the mixture was allowed to stir for another 1.5 hours. Finally the solvent was removed and the residue dissolved in 400 ml dichloromethane. This organic phase was washed two times with 500 ml NaHCO3 solution. The dichloromethane phase was dried then the solvent was evaporated. Purity of the product was judged by gas chromatography.

後処理

  1. stirringto stir for another 1.5 hours
  2. customFinally the solvent was removed
  3. dissolutionthe residue dissolved in 400 ml dichloromethane
  4. washThis organic phase was washed two times with 500 ml NaHCO3 solution
  5. dry with materialThe dichloromethane phase was dried
  6. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-457a9135c9e34ee6b321e781a6b88108
出典データセット
uspto-grants-2016_03
特許番号
US09283186B2

関連ノート

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