Morpholine → 4-[5-Chloro-4-[(4-chlorophenylthio)-(2,5-difluorophenyl)methyl]pyridin-2-yl]morpholine

HRID 2080398ノート

反応式

HRID 2080398 の反応式
O1CCOCC1.Cl[C:8]1[CH:13]=[C:12]([CH:14]([S:23][C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=2)[C:15]2[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:16]=2[F:22])[C:11]([Cl:31])=[CH:10][N:9]=1.[NH:32]1[CH2:37][CH2:36][O:35][CH2:34][CH2:33]1>C(OCC)(=O)C>[Cl:31][C:11]1[C:12]([CH:14]([S:23][C:24]2[CH:25]=[CH:26][C:27]([Cl:30])=[CH:28][CH:29]=2)[C:15]2[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:16]=2[F:22])=[CH:13][C:8]([N:32]2[CH2:37][CH2:36][O:35][CH2:34][CH2:33]2)=[N:9][CH:10]=1

参加物

5

反応物 3

HCID 8083MorpholineHCID 312751,4-DioxaneHCID 231145672,5-Dichloro-4-[(4-chlorophenylthio)-(2,5-difluorophenyl)methyl]pyridine

生成物 1

HCID 231147414-[5-Chloro-4-[(4-chlorophenylthio)-(2,5-difluorophenyl)methyl]pyridin-2-yl]morpholine収率 89%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A 1,4-dioxane (1.0 ml) solution of the 2,5-dichloro-4-[(4-chlorophenylthio)-(2,5-difluorophenyl)methyl]pyridine (100 mg, 0.24 mmol) obtained in Example 54 and morpholine (200 μl) was stirred at 100° C. for 2 days under a nitrogen atmosphere. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate (40 ml). The diluted mixture was washed with water and brine, dried and then concentrated under reduced pressure to give a residue. The resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=5:1) to give the title compound (100 mg, 89%) as an oil.

後処理

  1. washThe diluted mixture was washed with water and brine
  2. customdried
  3. concentrationconcentrated under reduced pressure
  4. customto give a residue
  5. customThe resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-9ee5c21a52fc454083722ca80d108027
出典データセット
uspto-grants-2011_04
特許番号
US07932271B2

反応ノート

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