Methanol → 2-Methyl-1-propyl-1,3-benzodiazole-5-carboxylic acid

HRID 74261

반응식

HRID 74261 반응식
CO.[NH2:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[NH:13][CH2:14][CH2:15][CH3:16])[C:7]([OH:9])=[O:8].Cl.[C:18](=N)(OC)[CH3:19]>C(OCC)C>[CH3:18][C:19]1[N:13]([CH2:14][CH2:15][CH3:16])[C:12]2[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][C:4]=2[N:3]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 115864403-Amino-4-(propylamino)benzoic acid

생성물 1

HCID 202988562-Methyl-1-propyl-1,3-benzodiazole-5-carboxylic acid수율 116.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a methanol (17 mL) solution of 3-amino-4-n-propylaminobenzoic acid (see Working Example 82-2) (1.68 g, 8.65 mmol) was added methyl acetimidate hydrochloride (1.14 g, 10.4 mmol), and this was heated to reflux for 4 hours. After the reaction was complete, this was cooled to room temperature, diethyl ether was added, and this was allowed to stand at room temperature for 10 minutes. The crystals obtained were filtered, and after being washed with diethyl ether, they were dried to yield the title compound (2.20 g, quant.).

후처리

  1. temperaturethis was heated
  2. temperatureto reflux for 4 hours
  3. customThe crystals obtained
  4. filtrationwere filtered
  5. washafter being washed with diethyl ether, they
  6. customwere dried

출처 및 근거

ORD 기록
ord-3eb052daec9a47e6839ab79527356e8e
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

연결된 노트

불러오는 중…