Phenothiazine → Diethyl allylphosphonate

HRID 328543

反応式

HRID 328543 の反応式
[P:1]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])[O:2]CC.[CH:11]1[C:24]2NC3C(=CC=CC=3)SC=2C=C[CH:12]=1.C(Cl)C=C>[Co]>[CH2:9]([O:8][P:1]([CH2:24][CH:11]=[CH2:12])(=[O:2])[O:5][CH2:6][CH3:7])[CH3:10]

参加物

5

反応物 3

HCID 7108PhenothiazineHCID 7850Allyl chlorideHCID 31215Triethyl phosphite

生成物 1

HCID 573014Diethyl allylphosphonate

試薬・触媒・溶媒 1

HCID 104730Cobalt触媒

実験手順

166 parts of triethyl phosphite are heated for 1 hour to 140° C in a nitrogen atmosphere with 2 parts of highly active Raney cobalt (Ra-Co-Lu). A mixture of 1 part of phenothiazine and 80 parts of allyl chloride is then added dropwise at 140° C. Once the reaction has started, the temperature may be lowered to 120° C. After 5.5 hours, 63 parts of ethyl chloride have distilled off and the mixture is deep blue in colour. Fractional distillation gives 135 parts of allyl phosphonic acid diethyl ester, corresponding to 76% of the theoretical yield.

後処理

  1. additionis then added dropwise at 140° C
  2. custommay be lowered to 120° C
  3. distillation63 parts of ethyl chloride have distilled off
  4. distillationFractional distillation

出典と根拠

ORDレコード
ord-d23f6875737846dd9075b4bb91fd9f56
出典データセット
uspto-grants-1977_04
特許番号
US04017564

関連ノート

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