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Diglyme → HCID 23455911, 화합물

HRID 1702848
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HRID 1702848 반응식
[F:1][C:2]([F:10])([F:9])[C:3]([C:5]([F:8])([F:7])[F:6])=[O:4].[F-:11].[K+].COCCOCCOC.Cl[C:23]([F:30])([F:29])[C:24]([Cl:28])=[C:25]([F:27])[F:26]>O>[F:11][C:3]([O:4][C:23]([F:30])([F:29])[C:24]([Cl:28])=[C:25]([F:27])[F:26])([C:5]([F:8])([F:7])[F:6])[C:2]([F:10])([F:9])[F:1]
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HCID 8150Diglyme2회HCID 12695HexafluoroacetoneHCID 522689Potassium FluorideHCID 125650472,3-Dichloro-1,1,3,3-tetrafluoroprop-1-ene

생성물 1

HCID 23455911HCID 23455911, 화합물수율 39%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Hexafluoroacetone (16.6 g, 0.10 mol) was distilled into a stirred mixture of potassium fluoride (5.80 g, 0.10 mol) and 1-(2-methoxyethoxy)-2-methoxyethane (hereinafter referred to as diglyme) (100 ml) to give a homogeneous solution. This mixture was maintained at 25°-30° C. and treated with 1,2-dichloro-1,1,3,3-tetrafluoropropene (18.3 g, 0.10 mol, prepared according to J. E. Bissey, H. Goldwhite and D. G. Rowsell, J. Org. Chem., 32, 1542 (1967)). The mixture was stirred overnight and then it was poured into water (500 ml). The lower layer was washed with water (250 ml), dried, and distilled to give 1-(heptafluoro-2-propoxy)-1,1,3,3-tetrafluoro-2-chloropropene (13.0 g, 0.039 mol, 39%), bp 82°-83° C. whose structure was confirmed by the following: λmax 5.72 (CCl=CF2) and 7.5-10 μm (CF, C--O); 19F NMR, -64.9 (m) 2F, --OCF2C=C; -76.0 (2nd order m) 2F, C=CF2 ; -81.2 t J=5.7 Hz, each member d J=2.2 Hz) 6F, CF3 ; and -146.7 ppm (t J=22.9 Hz each member septet J=2.2 Hz) 1F, CFO.

후처리

  1. customto give a homogeneous solution
  2. temperatureThis mixture was maintained at 25°-30° C.
  3. washThe lower layer was washed with water (250 ml)
  4. customdried
  5. distillationdistilled

출처 및 근거

ORD 기록
ord-9cbba7e0d9e64b49bd9041a27a84262d
출처 데이터셋
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04349650

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