Sodium Hydroxide → HCID 178488129、化合物

HRID 1655230ノート

反応式

HRID 1655230 の反応式
[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

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 197911192-Chloromethyl-3-fluoro-4-morpholinopyridine hydrochlorideHCID 178488140HCID 178488140、化合物

生成物 1

HCID 178488129HCID 178488129、化合物収率 74.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-b6b5e8f4a10a43efaa1a534c3602f7ba
出典データセット
uspto-grants-1993_10
特許番号
US05250527

反応ノート

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