Ammonia → HCID 70314200, 화합물

HRID 1713934

반응식

HRID 1713934 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10]([O:12][CH3:13])=[O:11])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].[NH3:17]>CS(C)=O>[NH2:17][C:2]1[CH:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10]([O:12][CH3:13])=[O:11])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 28818827methyl (2E)-3-(4-chloro-3-nitrophenyl)prop-2-enoate

생성물 1

HCID 70314200HCID 70314200, 화합물수율 89%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of methyl (2E)-3-(4-chloro-3-nitrophenyl)acrylate (from Step 1, 1 eq) in DMSO (0.4 M) at 140° C., ammonia gas was bubbled through for 6 h. The reaction mixture was cooled to RT, degassed with nitrogen, and poured into ice cold water. The precipitate formed was filtered washed with cold water and dried under vacuo to afford the title compound (89%) as a solid. 1H-NMR (400 MHz; DMSO-d6, 300 K) δ 3.70, (s, 3H), 6.46 (d, J 16, 1H), 7.04 (d, J 8.8, 1H), 7.60 (d, J 16, 1H), 7.82-7.86 (m, 3H), 8.25 (s, 1H); MS (ES−) m/z 221 (M−H)−.

후처리

  1. customdegassed with nitrogen
  2. additionpoured into ice cold water
  3. customThe precipitate formed
  4. filtrationwas filtered
  5. washwashed with cold water
  6. customdried under vacuo

출처 및 근거

ORD 기록
ord-001828ea21dc4f8aac82d7cabbf32822
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795250B2

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