Dichloromethane → HCID 86584678、化合物

HRID 279483ノート

反応式

HRID 279483 の反応式
[H-].C([Al+]CC(C)C)C(C)C.C1(C)C=CC=CC=1.[CH3:18][C:19](=[N:30][O:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[C:38](=[N:43][O:44][CH3:45])[C:39](OC)=[O:40])[C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=1.ClCCl>CO>[CH3:18][C:19](=[N:30][O:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[C:38](=[N:43][O:44][CH3:45])[CH:39]=[O:40])[C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:28])([F:29])[F:27])[CH:21]=1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 86583787Diisobutylaluminumhydride tolueneHCID 86584679HCID 86584679、化合物

生成物 1

HCID 86584678HCID 86584678、化合物収率 49.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1M diisobutylaluminum hydride/toluene solution (11 ml, 16.5 mmol) was added dropwise to a mixture of methyl 2-[(α-methyl-3-trifluoromethylbenzylidene)aminooxy]-α-methoxyiminophenylacetate (4.83 g, 11.8 mmol) and dichloromethane (47 ml) at −65° C. or lower over 4 minutes, and the mixture was stirred at −78° C. to room temperature for 3 hours. Methanol (7 ml) was added to the reaction mixture, and the mixture was stirred at room temperature for 1 hour. The precipitated insoluble materials were removed, and the remaining mixture was concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to give 2-[(α-methyl-3-trifluoromethylbenzylidene)aminooxy]-α-methoxyiminophenylacetaldehyde (2.11 g, 47.3%) as a colorless

後処理

  1. stirringthe mixture was stirred at room temperature for 1 hour
  2. customThe precipitated insoluble materials were removed
  3. concentrationthe remaining mixture was concentrated under reduced pressure
  4. customThe residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-15c4c7f5430e4cc5b56762072cbb046d
出典データセット
uspto-grants-2002_03
特許番号
US06362212B1

反応ノート

読み込み中…