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N,N-Dimethylglycine → N-(2-(2,5-Dimethyl-1-pyrrolyl)ethyl)-(N,N-dimethylamino)acetamide

HRID 1904229
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HRID 1904229 반응식
[CH3:1][N:2]([CH2:4][C:5]([OH:7])=O)[CH3:3].C(N1C=CN=C1)(N1C=CN=C1)=O.[NH2:20][CH2:21][CH2:22][N:23]1[C:27]([CH3:28])=[CH:26][CH:25]=[C:24]1[CH3:29]>COCCOC>[CH3:29][C:24]1[N:23]([CH2:22][CH2:21][NH:20][C:5](=[O:7])[CH2:4][N:2]([CH3:3])[CH3:1])[C:27]([CH3:28])=[CH:26][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 673N,N-DimethylglycineHCID 682631,1'-CarbonyldiimidazoleHCID 137700502-(2,5-Dimethyl-1H-pyrrol-1-yl)ethan-1-amine

생성물 1

HCID 13770064N-(2-(2,5-Dimethyl-1-pyrrolyl)ethyl)-(N,N-dimethylamino)acetamide

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

5.2 g (0.05 mol) of N,N-dimethylaminoacetic acid and 8.1 g (0.05 mol) of carbonyldiimidazole in 20 ml of ethylene glycol dimethyl ether are stirred at 70° C. for 15 min. After addition of 5.5 g (0.04 mol) of 1-(2-aminoethyl)-2,5-dimethylpyrrole, dissolved in 20 ml of ethylene glycol dimethyl ether, to the mixture it is stirred at room temperature for 5 h, then concentrated, water is added, and the mixture is extracted first when acid and then when alkaline. The product contained in the extract from the mixture which has been made alkaline is crystallized using ligroin. Yield: 4.3 g (39% of theory), Melting point: 63°-65° C. Elemental analysis: C12H21N3O (223.32) calculated: C 64.5 H 9.5 N 18.8 O 7.2 found: C 64.0 H 9.4 N 18.5 O 8.0

후처리

  1. concentrationconcentrated
  2. additionwater is added
  3. extractionthe mixture is extracted first when acid
  4. extractionextract from the mixture which
  5. customis crystallized

출처 및 근거

ORD 기록
ord-732bc9f7c96643e3aa7eb9ec59007b2f
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04837225

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