Dimethyl Sulfoxide → HCID 67534545、化合物

HRID 1943538ノート

反応式

HRID 1943538 の反応式
C(Cl)(=O)C(Cl)=O.CS(=O)C.[O:11]=[P:12]1([CH2:26][OH:27])[C:25]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[O:13]1>C(N(CC)CC)C>[O:11]=[P:12]1([CH:26]=[O:27])[C:25]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[O:13]1

参加物

5

反応物 3

HCID 679Dimethyl SulfoxideHCID 65578Oxalyl chlorideHCID 146868856-(Hydroxymethyl)-6H-6lambda~5~-dibenzo[c,e][1,2]oxaphosphinin-6-one2 回

生成物 1

HCID 67534545HCID 67534545、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

Purified dichloro methane anhydride 100 ml is cooled using dry ice and acetone. When the cooling is completed, oxalyl chloride 42.5 ml (0.05 mol) and dimethyl sulfur oxide 5.76 ml (0.08 mol) are added. Thereafter, they are stirred for 10 minutes. Then, (10-oxo-10H-9-oxa-10-phosphaphenanthrene-10-yl)-methanol (compound F) 10 g (0.04 mol) is added thereto. Thereafter, they are stirred for 1 hour. Then, triethylamine 22 ml is slowly added thereto. Thereafter, they are stirred at a normal temperature for 12 hours. When the reaction is completed, distilled water 100 ml is added thereto. Thereafter, solution is extracted using dichloro methane. The extracted solution is processed using 1N-hydrochloric acid water, saturated sodium bicarbonate solution, saturated brine water, or the like, and is dried using magnesium sulfate anhydride. The dried solution is filtered under reduced pressure and evaporated under reduced pressure to obtain brown solution. The obtained product is used for reaction in immediately subsequent step.

後処理

  1. customPurified dichloro methane anhydride 100 ml
  2. temperatureis cooled
  3. stirringThereafter, they are stirred for 1 hour
  4. stirringThereafter, they are stirred at a normal temperature for 12 hours
  5. distillationdistilled water 100 ml
  6. additionis added
  7. extractionThereafter, solution is extracted
  8. customthe like, and is dried
  9. filtrationThe dried solution is filtered under reduced pressure
  10. customevaporated under reduced pressure
  11. customto obtain brown solution
  12. customThe obtained product is used for reaction in immediately subsequent step

出典と根拠

ORDレコード
ord-11fba0dd485142c19aa1d388e21281c2
出典データセット
uspto-grants-2013_03
特許番号
US08394512B2

反応ノート

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