1,1-Dichloro-2,2-difluoroethene → Benzene, 1-(2,2-dichloro-3,3-difluorocyclobutyl)-4-methoxy-

HRID 258959

反応式

HRID 258959 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[CH2:8])=[CH:5][CH:4]=1.[Cl:11][C:12]([Cl:16])=[C:13]([F:15])[F:14].C(N(CC)CC)C>O>[Cl:11][C:12]1([Cl:16])[CH:7]([C:6]2[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH2:8][C:13]1([F:15])[F:14]

参加物

5

反応物 3

HCID 65921,1-Dichloro-2,2-difluoroetheneHCID 8471TriethylamineHCID 125074-Methoxystyrene

生成物 1

HCID 21425195Benzene, 1-(2,2-dichloro-3,3-difluorocyclobutyl)-4-methoxy-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

p-Methoxystyrene (40.8 g., 0.30 mole), 1,1-dichloro-2,2-difluoroethylene (55.8 g., 0.42 mole), and triethylamine (3.0 ml., 0.02 mole) are heated in a sealed tube (25 × 615 mm) at 125°-130° C. for 16 hrs. The cooled mixture is then poured into water, the reaction product extracted with ether, and the extracts washed with water, dried (MgSO4), and evaporated to an oil. Distillation of the oil yields 69.0 g. (86%), b.p. 80°-85° C. (0.1 mm), of the desired intermediate sutiable for use in the next step. Part of the oil was chromatographed (alumina, cyclohexane), and redistilled, b.p. 81° C. (0.02 mm), nD27 1.5207.

後処理

  1. extractionthe reaction product extracted with ether
  2. washthe extracts washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated to an oil
  5. distillationDistillation of the oil
  6. customyields 69.0 g
  7. customPart of the oil was chromatographed (alumina, cyclohexane)
  8. distillationredistilled

出典と根拠

ORDレコード
ord-38d988b8ebe3450c9217832735ceadc0
出典データセット
uspto-grants-1977_07
特許番号
US04035426

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