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Dimethylamine → HCID 21514639、化合物

HRID 1576140
ノート
印刷プレビュー

反応式

HRID 1576140 の反応式
[CH3:1][C:2]([NH:8][C:9](=[O:14])[CH2:10][CH2:11][O:12][CH3:13])([CH3:7])[CH2:3][C:4](=O)[CH3:5].[CH3:15][NH:16][CH3:17].Cl([O-])(=O)(=O)=O.C[NH2+]C.[H][H].C(=O)(O)[O-].[Na+]>[Pt]=O>[CH3:1][C:2]([NH:8][C:9](=[O:14])[CH2:10][CH2:11][O:12][CH3:13])([CH3:7])[CH2:3][CH:4]([N:16]([CH3:17])[CH3:15])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 674DimethylamineHCID 516892Sodium BicarbonateHCID 14786861HCID 14786861、化合物HCID 21514640HCID 21514640、化合物HCID 178418361HCID 178418361、化合物3 回

生成物 1

HCID 21514639HCID 21514639、化合物

試薬・触媒・溶媒 1

HCID 82844
Platinum oxide (PtO)
触媒

実験手順

A one-gallon autoclave, fitted with a stirrer, is charged with 1684 parts (8.38 moles) of N-(1,1-dimethyl-3-oxobutyl)-3-methoxypropionamide, 762 parts (16.9 moles) of dimethylamine, 1.5 parts of platinum oxide and 15 parts of dimethylammonium perchlorate. The autoclave is pressurized with hydrogen to 750 psi., and stirring is begun. Hydrogen pressure is periodically restored to 850-900 psi. and stirring is continued until hydrogen uptake has ceased. Sodium bicarbonate, 10 parts, is added to the mixture which is then stripped, acidified, extracted with chloroform, made alkaline and again extracted with chloroform. The chloroform extract from the alkaline solution is stripped and distilled, and the product, N-(1,1-dimethyl-3-dimethylaminobutyl)-3-methoxypropionamide, is obtained boiling at 108°C./0.9 mm.

後処理

  1. customA one-gallon autoclave, fitted with a stirrer
  2. stirringand stirring
  3. extractionextracted with chloroform
  4. extractionagain extracted with chloroform
  5. extractionThe chloroform extract from the alkaline solution
  6. distillationdistilled

出典と根拠

ORDレコード
ord-c97949366565484ea93b505adbbec5d5
出典データセット
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03979441

反応ノート

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