Sodium Hydroxide → HCID 178488129, 화합물

HRID 1655230노트

반응식

HRID 1655230 반응식
[OH-].[Na+].Cl.Cl[CH2:5][C:6]1[C:11]([F:12])=[C:10]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)[CH:9]=[CH:8][N:7]=1.[CH3:19][O:20][C:21]1[CH:30]=[CH:29][C:24]2[NH:25][C:26]([SH:28])=[N:27][C:23]=2[CH:22]=1>C(O)C>[O:16]1[CH2:17][CH2:18][N:13]([C:10]2[CH:9]=[CH:8][N:7]=[C:6]([CH2:5][S:28][C:26]3[NH:25][C:24]4[CH:29]=[CH:30][C:21]([O:20][CH3:19])=[CH:22][C:23]=4[N:27]=3)[C:11]=2[F:12])[CH2:14][CH2:15]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 197911192-Chloromethyl-3-fluoro-4-morpholinopyridine hydrochlorideHCID 178488140HCID 178488140, 화합물

생성물 1

HCID 178488129HCID 178488129, 화합물수율 74.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

5N NaOH (3.39 ml) was added dropwise to a stirred solution of 2-chloromethyl-3-fluoro-4-morpholinopyridine hydrochloride (2.06 g) and 5-methoxy-(1H)-benzimidazole-2-thiol (1.39 g) in ethanol (35 ml). After 3 hours excess solvent was removed and the residue treated with water (80 ml) and extracted with dichloromethane. The extracts were washed with water, dried (K2CO3), excess solvent removed and the residue crystallised from ethyl acetate to yield 2-(4-morpholino-3-fluoro-2-pyridylmethylthio)-5-methoxy-(1H)-benzimidazole (2.16 g) m.p. 121°-123°.

후처리

  1. customAfter 3 hours excess solvent was removed
  2. additionthe residue treated with water (80 ml)
  3. extractionextracted with dichloromethane
  4. washThe extracts were washed with water
  5. dry with materialdried (K2CO3), excess solvent
  6. customremoved
  7. customthe residue crystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-b6b5e8f4a10a43efaa1a534c3602f7ba
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250527

반응 노트

불러오는 중…