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(E)-1,3-Dichloropropene → (E)-2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(3-chloroprop-2-enyloxy)pyridine

HRID 23318
ノート
印刷プレビュー

反応式

HRID 23318 の反応式
[OH:1][C:2]1[N:7]=[C:6]([O:8][C:9]2[N:13]([CH3:14])[N:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=2)[CH:5]=[C:4]([CH3:19])[CH:3]=1.[H-].[Na+].[Cl:22]/[CH:23]=[CH:24]/[CH2:25]Cl>C(#N)C.CN(C=O)C.CCCCC.C(OCC)(=O)C>[CH3:14][N:13]1[C:9]([O:8][C:6]2[CH:5]=[C:4]([CH3:19])[CH:3]=[C:2]([O:1][CH2:25]/[CH:24]=[CH:23]/[Cl:22])[N:7]=2)=[CH:10][C:11]([C:15]([F:18])([F:17])[F:16])=[N:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 24726(E)-1,3-DichloropropeneHCID 24758Sodium hydride2 回HCID 178429419HCID 178429419、化合物

生成物 1

HCID 15477174(E)-2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(3-chloroprop-2-enyloxy)pyridine収率 52.3%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒
HCID 6342
Acetonitrile
溶媒
HCID 22335286Ethyl acetate pentane溶媒

実験手順

A mixture of 6-hydroxy-2-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methylpyridine (0.9 g, 3.3 mmol) and NaH (60% in oil, 0.16 g, 4 mmol) in acetonitrile (20 ml) and DMF (1 ml) is stirred for 10 min at ambient temperature and (E)-1,3-dichloropropene (0.4 g, 3.6 mmol) is added. After stirring for 60 h at ambient temperature, the remaining NaH is deactivated and the resulting mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (0.6 g, 52% yield) as an colorless oil.

後処理

  1. stirringAfter stirring for 60 h at ambient temperature
  2. filtrationfiltered through a bed of silica gel
  3. washThe filtrate is washed with water
  4. dry with materialThe organic layer is dried with anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customPurification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v)

出典と根拠

ORDレコード
ord-1a51b45be5a940eea36ea661e6865feb
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06852673B2

反応ノート

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