Water → 5-(Benzoxazol-2-yl)-2-methyl-1-(tetrahydropyran-4-yl)-6-chlorobenzimidazole

HRID 74296노트

반응식

HRID 74296 반응식
[Cl:1][C:2]1[C:8]([C:9]2[O:10][C:11]3[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=3[N:13]=2)=[CH:7][C:5]([NH2:6])=[C:4]([NH:18][CH:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[CH:3]=1.Cl.[C:26](=N)(OC)[CH3:27].O>CO>[O:10]1[C:11]2[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=2[N:13]=[C:9]1[C:8]1[C:2]([Cl:1])=[CH:3][C:4]2[N:18]([CH:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[C:26]([CH3:27])=[N:6][C:5]=2[CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 67498666HCID 67498666, 화합물

생성물 1

HCID 674990465-(Benzoxazol-2-yl)-2-methyl-1-(tetrahydropyran-4-yl)-6-chlorobenzimidazole수율 79%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-(4-chloro-2-(tetrahydropyran-4-yl)aminoanilin-5-yl)benzoxazole (see Working Example 112-3) (0.04 g, 0.2 mmol) in methanol (1.2 mL) was added methyl acetimidate hydrochloride (0.06 g, 0.6 mmol), and this was heated to reflux for 3 hours. After the reaction solution was cooled, water was added, and the precipitated crystals were filtered, and after being washed with water were dried to yield the title compound (0.03 g, 79% yield) as a yellowish-brown solid.

후처리

  1. temperaturethis was heated
  2. temperatureto reflux for 3 hours
  3. temperatureAfter the reaction solution was cooled
  4. filtrationthe precipitated crystals were filtered
  5. washafter being washed with water
  6. customwere dried

출처 및 근거

ORD 기록
ord-64fdf773b4be4b79bf36b465f00207e1
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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