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Potassium Carbonate → 4-{2,6-Dichloro-4-[(3,3-dichloroprop-2-EN-1-YL)oxy]phenoxy}butan-1-OL

HRID 1611457
ノート
印刷プレビュー

反応式

HRID 1611457 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([OH:15])[CH:5]=[C:6]([Cl:14])[C:7]=1[O:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13].[Cl:16][C:17](Cl)([Cl:21])[CH2:18][CH2:19]Cl.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:16][C:17]([Cl:21])=[CH:18][CH2:19][O:15][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13])=[C:6]([Cl:14])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 140561,1,1,3-TetrachloropropaneHCID 222571313,5-Dichloro-4-(4-hydroxybutoxy)phenol

生成物 1

HCID 222571304-{2,6-Dichloro-4-[(3,3-dichloroprop-2-EN-1-YL)oxy]phenoxy}butan-1-OL収率 61.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

This compound was prepared in a manner analogous to that of Step D of Example 1, using 9.3 grams (0.036 mole) of 3,5-dichloro-4-(4-hydroxybutoxy)phenol, 7.7 grams (0.042 mole) of 1,1,1,3-tetrachloropropane and 11.7 grams (0.080 mole) of potassium carbonate in 300 mL of DMF. The crude product was purified with column chromatography on silica gel using mixtures of 1:4 and 1:1 ethyl acetate and hexane as eluants. The appropriate fractions were combined and concentrated under reduced pressure, yielding 8.0 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.

後処理

  1. customThis compound was prepared in a manner analogous to that of Step D of Example 1
  2. customThe crude product was purified with column chromatography on silica gel using mixtures of 1:4 and 1:1 ethyl acetate and hexane as eluants
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3c6c271c56bf415e95f6318cb100f9e8
出典データセット
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06987194B2

反応ノート

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