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Dimethylamine → HCID 21514639, 화합물

HRID 1576140
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HRID 1576140 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 674DimethylamineHCID 516892Sodium BicarbonateHCID 14786861HCID 14786861, 화합물HCID 21514640HCID 21514640, 화합물HCID 178418361HCID 178418361, 화합물3회

생성물 1

HCID 21514639HCID 21514639, 화합물

시약·촉매·용매 1

HCID 82844
Platinum oxide (PtO)
촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c97949366565484ea93b505adbbec5d5
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03979441

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