1,1,1-Trichloro-2,2,2-trifluoroethane → HCID 23282361、化合物

HRID 369689

反応式

HRID 369689 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)[C:26](F)([F:28])[F:27].[Cl-].[Al+3].[Cl-].[Cl-]>CN(C)C=O.[Zn]>[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:24])=[C:26]([F:28])[F:27]

参加物

6

反応物 3

HCID 96351,1,1-Trichloro-2,2,2-trifluoroethaneHCID 6451240Aluminum(III) ChlorideHCID 538269084-(2,6-Dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde

生成物 1

HCID 23282361HCID 23282361、化合物収率 38%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 6228Dimethylformamide溶媒

実験手順

Then, 19.54 g of 4-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde was dissolved in 200 ml of N,N-dimethylformamide, to which 25.3 g of 1,1,1-trichlorotrifluoroethane, 17.6 g of zinc dust and 2.0 g of aluminum chloride were added. After stirring at room temperature for 1.5 hours, the reaction mixture was filtered. The filtrate was poured into diluted hydrochloric acid and extracted twice with diethyl ether. The diethyl ether layers were combined, washed with water, dried over magnesium sulfate and then concentrated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 8.46 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-4,4-difluoro-2-hydoxy-3-butenyloxy)butyloxy)benzene (yield, 38%), nD22.5 1.5302.

後処理

  1. additionwere added
  2. filtrationthe reaction mixture was filtered
  3. additionThe filtrate was poured into diluted hydrochloric acid
  4. extractionextracted twice with diethyl ether
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated
  8. customto give a crude product

出典と根拠

ORDレコード
ord-44e24706c43649f8978e8ee0a1e5db3f
出典データセット
uspto-grants-2000_10
特許番号
US06140274

関連ノート

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