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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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1,1,1-Trichloro-2,2,2-trifluoroethane → 3,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-4,4,4-trifluoro-2-hydroxybutyloxy)butyloxy)benzene

HRID 369667
ノート
印刷プレビュー

反応式

HRID 369667 の反応式
[Cl:1][C:2]1[CH:16]=[C:15]([O:17][CH2:18][CH:19]=[C:20]([Cl:22])[Cl:21])[CH:14]=[C:13]([Cl:23])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][CH2:10][CH:11]=[O:12].[Cl:24][C:25](Cl)([Cl:30])[C:26]([F:29])([F:28])[F:27]>[Zn].CN(C)C=O>[Cl:1][C:2]1[CH:16]=[C:15]([O:17][CH2:18][CH:19]=[C:20]([Cl:22])[Cl:21])[CH:14]=[C:13]([Cl:23])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][CH2:10][CH:11]([OH:12])[C:25]([Cl:30])([Cl:24])[C:26]([F:29])([F:28])[F:27]
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 2

HCID 96351,1,1-Trichloro-2,2,2-trifluoroethaneHCID 538269084-(2,6-Dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde

生成物 1

HCID 232824133,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-4,4,4-trifluoro-2-hydroxybutyloxy)butyloxy)benzene収率 63.4%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 6228
Dimethylformamide
溶媒

実験手順

To a mixture of 2.01 g of 4-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde, 1.31 g of zinc dust and 10 ml of N,N-dimethylformamide was added 4.12 g of 1,1,1-trichlorotrifluoroethane. After stirring at room temperature for 1.5 hours, the reaction mixture was filtered. The filtrate was poured into 20 ml of diluted hydrochloric acid and extracted twice with 50 ml of ethyl acetate. The ethyl acetate layers were combined, washed with water, dried over magnesium sulfate and then evaporated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 1.76 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-4,4,4-trifluoro-2-hydroxybutyloxy)butyloxy)benzene (yield, 63%), nD24.2 1.5188.

後処理

  1. filtrationthe reaction mixture was filtered
  2. additionThe filtrate was poured into 20 ml of diluted hydrochloric acid
  3. extractionextracted twice with 50 ml of ethyl acetate
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customto give a crude product

出典と根拠

ORDレコード
ord-0618dde99335441b96a472b8e46bca52
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06140274

反応ノート

読み込み中…

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