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Water → (Z)-3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-4,4,4-trifluoro-2-butenyloxy)butyloxy)benzene

HRID 369659
ノート
印刷プレビュー

反応式

HRID 369659 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([O:23][CH2:24][CH:25]=[C:26]([Cl:28])[Cl:27])[CH:5]=[C:6]([Cl:22])[C:7]=1[O:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH2:14][CH:15](O)[C:16]([Cl:20])=[C:17]([F:19])[F:18].C(N(S(F)(F)[F:35])CC)C.O>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([O:23][CH2:24][CH:25]=[C:26]([Cl:28])[Cl:27])[CH:5]=[C:6]([Cl:22])[C:7]=1[O:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH2:14]/[CH:15]=[C:16](\[Cl:20])/[C:17]([F:35])([F:19])[F:18]
参加物反応条件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 962WaterHCID 123472(Diethylamino)sulfur trifluorideHCID 232823613,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-4,4-difluoro-2-hydroxy-3-butenyloxy)butyloxy)benzene

生成物 1

HCID 23282399(Z)-3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-4,4,4-trifluoro-2-butenyloxy)butyloxy)benzene収率 55.3%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

反応条件

温度
-78 °C

実験手順

A solution of 0.36 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-4,4-difluoro-2-hydroxy-3-butenyloxy)butyloxy)benzene in 5 ml of dichloromethane was slowly added dropwise to a solution of 0.12 g of diethylaminosulfur trifluoride (DAST) in 10 ml of dichloromethane with stirring at -78° C. After complement of the dropwise addition, the reaction mixture was returned to room temperature over 30 minutes and poured into water. The dichloromethane layer was separated, 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 0.20 g of (Z)-3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-4,4,4-trifluoro-2-butenyloxy)butyloxy)benzene (yield, 55%), nD23.7 1.5160.

後処理

  1. additionAfter complement of the dropwise addition
  2. customThe dichloromethane layer was separated
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customto give a crude product

出典と根拠

ORDレコード
ord-70b956be9386450486f29221aba451ad
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…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート