1H-Pyrazol-3-amine, 5-methyl- → HCID 178486653, 화합물

HRID 2100754노트

반응식

HRID 2100754 반응식
[C:1]([CH2:3][C:4]1[C:9]([C:10](O)=[O:11])=[CH:8][C:7]([C:13]([N:15]([CH3:17])[CH3:16])=[O:14])=[C:6]([O:18][CH3:19])[CH:5]=1)#[N:2].[NH2:20][C:21]1[CH:25]=[C:24]([CH3:26])[NH:23][N:22]=1>C(O)(=O)C>[CH3:16][N:15]([CH3:17])[C:13]([C:7]1[CH:8]=[C:9]2[C:4]([CH:3]=[C:1]([NH:20][C:21]3[CH:25]=[C:24]([CH3:26])[NH:23][N:22]=3)[N:2]=[C:10]2[OH:11])=[CH:5][C:6]=1[O:18][CH3:19])=[O:14]

참가 물질

4

반응물 2

HCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 57799630HCID 57799630, 화합물

생성물 1

HCID 178486653HCID 178486653, 화합물수율 85%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
130 °C

실험 절차

A mixture of 6-Cyanomethyl-4-methoxy-N,N-dimethyl-isophthalamic acid (2.0 g, 7.6 mmol), 3-amino-5-methylpyrazol (1.5 g, 15.44 mmol), acetic acid (10 ml) were sealed in microwave process vial (20 ml). The mixture was heated at 130° C. for 30 minutes under microwave irradiation. After removal of acetic acid, the residue was dissolved in 1.5 ml MeOH, and this solution was added dropwise to 30 ml water. After stirred for 1 hour, the solid was collected and was purified by flash column chromatography to give product (2.2 g, 85%). LC-MS: m/e 342 (MH+).

후처리

  1. customwere sealed in microwave process vial (20 ml)
  2. customAfter removal of acetic acid
  3. dissolutionthe residue was dissolved in 1.5 ml MeOH
  4. additionthis solution was added dropwise to 30 ml water
  5. customthe solid was collected
  6. customwas purified by flash column chromatography

출처 및 근거

ORD 기록
ord-83135e71faa54c288857eb4bf2fc2bb0
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572809B2

반응 노트

불러오는 중…