1,1,3-Trichloropropene → 2-Trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene

HRID 260775

反応式

HRID 260775 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:8]=[C:7]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH3:18])[CH:11]=2)[CH:6]=[CH:5][C:4]=1[OH:19].[Cl:22][C:23]([Cl:27])=[CH:24][CH2:25]Cl>[H-].[Na+].CN(C)C=O>[F:1][C:2]([F:20])([F:21])[C:3]1[CH:8]=[C:7]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH3:18])[CH:11]=2)[CH:6]=[CH:5][C:4]=1[O:19][CH2:25][CH:24]=[C:23]([Cl:27])[Cl:22]

参加物

5

反応物 2

HCID 173781,1,3-TrichloropropeneHCID 214661922-Trifluoromethyl-4-(3-ethoxyphenoxy)phenol

生成物 1

HCID 214663272-Trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene収率 62%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 24758Sodium hydride溶媒

実験手順

To a solution prepared by dissolving 0.44 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)phenol in 10 ml of N,N-dimethylfonnamide, 0.062 g of sodium hydride (60% oil-based) was added with stirring under ice cooling. After 10 minutes, a solution prepared by dissolving 0.24 g of 1,1,3-trichloro-1-propene in 5 ml of N,N-dimethylformamide was added dropwise under ice cooling. After stirring at room temperature for 10 hours, the reaction solution was poured into ice-water, and extracted twice with 50 ml of diethyl ether. Then, the ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 0.37 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene, yield 62%; nD23.6 1.5369.

後処理

  1. customTo a solution prepared
  2. additionwas added
  3. customa solution prepared
  4. additionwas added dropwise under ice cooling
  5. stirringAfter stirring at room temperature for 10 hours
  6. extractionextracted twice with 50 ml of diethyl ether
  7. washwashed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationconcentrated
  10. customto give a crude product

出典と根拠

ORDレコード
ord-f65b3b2a15ee45b5af15143deb6dd724
出典データセット
uspto-grants-1996_06
特許番号
US05530015

関連ノート

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