Sodium Hydroxide → 5-Fluoro-2-[(4-methoxy-3-methyl-2-pyridyl)methylthio]benzimidazole

HRID 1709758노트

반응식

HRID 1709758 반응식
[F:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[C:7]([SH:9])[NH:8][C:4]=2[CH:3]=1.Cl.Cl[CH2:14][C:15]1[C:20]([CH3:21])=[C:19]([O:22][CH3:23])[CH:18]=[CH:17][N:16]=1.[OH-].[Na+]>O>[F:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[C:7]([S:9][CH2:14][C:15]3[C:20]([CH3:21])=[C:19]([O:22][CH3:23])[CH:18]=[CH:17][N:16]=3)[NH:8][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 34348855-Fluoro-1H-benzo[d]imidazole-2(3H)-thioneHCID 115139822-(Chloromethyl)-4-methoxy-3-methylpyridine--hydrogen chloride (1/1)

생성물 1

HCID 190244985-Fluoro-2-[(4-methoxy-3-methyl-2-pyridyl)methylthio]benzimidazole

시약·촉매·용매 1

HCID 962Water용매

실험 절차

10.6 g of 5-fluoro-2-benzimidazolethiol were suspended in 570 ml of alcohol and treated with 13.1 g of 2-chloromethyl-4-methoxy-3-methylpyridine hydrochloride. A solution of 5 g of sodium hydroxide in 130 ml of water was added dropwise thereto while cooling with ice, the mixture was left to boil at reflux overnight and then concentrated to about 1/3 of the volume in a vacuum. After the addition of 500 ml of water the resulting crystals were filtered off and washed thoroughly firstly with water and then with ether. There was obtained 5-fluoro-2-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]benzimidazole of melting point 128°.

후처리

  1. temperaturewhile cooling with ice
  2. waitthe mixture was left
  3. temperatureat reflux overnight
  4. concentrationconcentrated to about 1/3 of the volume in a vacuum
  5. additionAfter the addition of 500 ml of water the resulting crystals
  6. filtrationwere filtered off
  7. washwashed thoroughly firstly with water

출처 및 근거

ORD 기록
ord-8dafc7d0ea70437d80b012f503170dae
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04950677

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