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Methylamine → HCID 86340167, 화합물

HRID 2275007
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HRID 2275007 반응식
Cl[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[O:15][CH3:16].[CH3:17][NH2:18]>CN(C)C=O>[CH3:16][O:15][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N+:12]([O-:14])=[O:13])[C:2]=1[NH:18][CH3:17])[C:6]([O:8][CH3:9])=[O:7]
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 49757533Methyl 4-chloro-3-methoxy-5-nitrobenzoate

생성물 1

HCID 86340167HCID 86340167, 화합물수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

Methyl 4-chloro-3-methoxy-5-nitrobenzoate (available from, for example, Apollo Scientific Ltd) (14 g, 57.0 mmol) was dissolved in N,N-dimethylformamide (DMF) (140 mL) and cooled to ˜0° C. in an ice/water bath. Methanamine (2M in THF) (114 mL, 228 mmol) was added dropwise with vigorous stirring using a dropping funnel and the mixture was flushed with nitrogen and heated at 80° C. for 3 hr. The mixture was allowed to cool to room temperature over the weekend. The reaction mixture was diluted with water (500 mL), and filtered under vacuum to give the title compound as an orange solid (13.69 g).

후처리

  1. customthe mixture was flushed with nitrogen
  2. temperatureheated at 80° C. for 3 hr
  3. temperatureto cool to room temperature over the weekend
  4. additionThe reaction mixture was diluted with water (500 mL)
  5. filtrationfiltered under vacuum

출처 및 근거

ORD 기록
ord-2a29b6b84f7446af8cf239e56ed68698
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09127003B2

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