Water → HCID 59463314, 화합물

HRID 1712939노트

반응식

HRID 1712939 반응식
[Br:1][C:2]1[CH:10]=[CH:9][C:8]([N:11]([CH3:13])[CH3:12])=[CH:7][C:3]=1[C:4](O)=[O:5].C1N=C[N:16](C(N2C=NC=C2)=O)C=1.C(=O)([O-])[O-].[NH4+].[NH4+].O>CN(C=O)C>[Br:1][C:2]1[CH:10]=[CH:9][C:8]([N:11]([CH3:13])[CH3:12])=[CH:7][C:3]=1[C:4]([NH2:16])=[O:5]

참가 물질

6

반응물 4

HCID 962WaterHCID 682631,1'-CarbonyldiimidazoleHCID 517111Ammonium CarbonateHCID 53216701Benzoic acid, 2-bromo-5-(dimethylamino)-

생성물 1

HCID 59463314HCID 59463314, 화합물수율 27.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of give 2-bromo-5-(dimethylamino)benzoic acid (7.89 g, 32.3 mmol) in DMF (25 mL) was added N,N-carbonyldiimidazole (13.1 g, 80.8 mmol). The reaction mixture was allowed to stir at rt for 30 min and then ammonium carbonate (14.0 g, 145 mmol) was added. The reaction mixture was allowed to stir at rt overnight and then poured into water. The mixture was extracted with EtOAc. The organic solutions were combined, washed with water and brine, dried over Na2SO4, filtered and concentrated to give 2-bromo-5-(dimethylamino)benzamide (2.14 g, 27%). The product could be further purified by recrystallization from MeOH.

후처리

  1. stirringto stir at rt overnight
  2. extractionThe mixture was extracted with EtOAc
  3. washwashed with water and brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d6415d867c9a449a8b59602129532374
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795249B2

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