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

HRID 74296ノート

反応式

HRID 74296 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 67498666HCID 67498666、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-64fdf773b4be4b79bf36b465f00207e1
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

反応ノート

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