1,1-Dichloro-2,2-diethoxyethane → Chloroketene diethylacetal

HRID 1769060ノート

反応式

HRID 1769060 の反応式
[CH2:1]([O:3][CH:4]([O:8][CH2:9][CH3:10])[CH:5](Cl)[Cl:6])[CH3:2].CC(C)([O-])C.[K+]>C1COCC1>[Cl:6][CH:5]=[C:4]([O:8][CH2:9][CH3:10])[O:3][CH2:1][CH3:2]

参加物

4

反応物 2

HCID 120801,1-Dichloro-2,2-diethoxyethaneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 6451889Chloroketene diethylacetal収率 90%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of dichloroacetaldehyde diethylacetal (25 g; 0.1336 mol) in 150 ml of THF cooled to 0° C. was added 17.99 g (0.16 mol) of potassium t-butoxide in 50 ml of THF. The ice-bath was removed, and the reaction mixture was allowed to reflux for 16 hr and cooled. The reaction mixture was filtered (through celite) and a pale yellow solution was concentrated in vacuo at 30° C. The residue was distilled to afford 18.1 g (90%) of 2-chloro-1,1-diethoxyethylene (Formula V: R3 =Cl; R4 =H; R5 =R6 =OC2H5), a colorless liquid, b.p. 70°-76° C./20-25 mm.

後処理

  1. customThe ice-bath was removed
  2. temperatureto reflux for 16 hr
  3. temperaturecooled
  4. filtrationThe reaction mixture was filtered (through celite)
  5. concentrationa pale yellow solution was concentrated in vacuo at 30° C
  6. distillationThe residue was distilled

出典と根拠

ORDレコード
ord-d57971863345404fbfa30e2a65cd833f
出典データセット
uspto-grants-1995_01
特許番号
US05380729

反応ノート

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