Chloroform → HCID 21094281、化合物

HRID 1350073ノート

反応式

HRID 1350073 の反応式
[C:1]([CH:3]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=1)[C:4]([O:6][CH3:7])=[O:5])#[N:2].C(Cl)(Cl)[Cl:17]>CO.CCOCC.O=[Pt]=O>[ClH:17].[NH2:2][CH2:1][CH:3]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=1)[C:4]([O:6][CH3:7])=[O:5]

参加物

6

反応物 2

HCID 6212ChloroformHCID 69439208HCID 69439208、化合物

生成物 1

HCID 21094281HCID 21094281、化合物

試薬・触媒・溶媒 3

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

The compound obtained in Step A (34.32 g; 0.1672 mol) is dissolved in 150 ml of methanol. The solution is poured into an autoclave and then 50 ml of chloroform and platinium oxide (10% by weight) are added to the solution. The autoclave is placed under hydrogen pressure (60 bars) at ambient temperature and stirred magnetically for 24 hours. After removal of the catalyst by filtration, the solution is evaporated under reduced pressure. The oil obtained is taken up in ether. The precipitate formed is suction-filtered off and recrystallised from acetonitrile to yield the title product in the form of a white solid.

後処理

  1. additionThe solution is poured into an autoclave
  2. customat ambient temperature
  3. customAfter removal of the catalyst
  4. filtrationby filtration
  5. customthe solution is evaporated under reduced pressure
  6. customThe oil obtained
  7. customThe precipitate formed
  8. filtrationis suction-filtered off
  9. customrecrystallised from acetonitrile

出典と根拠

ORDレコード
ord-5b8111009f8342d1b81da58aa1532995
出典データセット
uspto-grants-2007_05
特許番号
US07214689B2

反応ノート

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