Dimethylformamide dimethyl acetal → Methyl 4-ethoxy-5-methoxy-2-(dimethylaminomethyleneamino)benzoate

HRID 612116

반응식

HRID 612116 반응식
[NH2:1][C:2]1[CH:11]=[C:10]([O:12][CH2:13][CH3:14])[C:9]([O:15][CH3:16])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].CO[CH:19](OC)[N:20]([CH3:22])[CH3:21]>CN(C=O)C.CC(N(C)C)=O>[CH2:13]([O:12][C:10]1[C:9]([O:15][CH3:16])=[CH:8][C:3]([C:4]([O:6][CH3:7])=[O:5])=[C:2]([N:1]=[CH:19][N:20]([CH3:22])[CH3:21])[CH:11]=1)[CH3:14]

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 10489373Methyl 2-amino-4-ethoxy-5-methoxybenzoate

생성물 1

HCID 10779127Methyl 4-ethoxy-5-methoxy-2-(dimethylaminomethyleneamino)benzoate수율 97.1%

시약·촉매·용매 1

HCID 22628260N,N-dimethylformamide N,N-dimethylacetamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 15.056 g (66.9 mmol) methyl 2-amino-4-ethoxy-5-methoxybenzoate and 14.1 ml (100 mmol) N,N-dimethylformamide dimethylacetal was heated to 100° C. under N2. At 4.5 hours added 4.7 ml (33.3 mmol) more DMF/DMA and removed heat at 5 hours. Stripped solvent, azeotroped with toluene, and dried in vacuo, giving 18.211 g of grey-brown solid: mass spectrum (electrospray m/e): M+H=281.3.

후처리

  1. customremoved
  2. temperatureheat at 5 hours
  3. customStripped solvent, azeotroped with toluene
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-b625d53183804ba2bb7b702fdf150b11
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06002008

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