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

HRID 2080398노트

반응식

HRID 2080398 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9ee5c21a52fc454083722ca80d108027
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932271B2

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