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(4-Cyano-3-fluorophenyl)[1-(triphenylmethyl)imidazol-4-yl]methanol → 4-Cyano-3-fluorophenyl 1-(triphenylmethyl)imidazol-4-yl ketone

HRID 278183
ノート
印刷プレビュー

反応式

HRID 278183 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:11]2[N:12]=[CH:13][N:14]([C:16]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:15]=2)[OH:10])=[CH:5][C:4]=1[F:35])#[N:2]>C(Cl)Cl.O=[Mn]=O>[C:29]1([C:16]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[N:14]2[CH:15]=[C:11]([C:9]([C:6]3[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[C:4]([F:35])[CH:5]=3)=[O:10])[N:12]=[CH:13]2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 11134299(4-Cyano-3-fluorophenyl)[1-(triphenylmethyl)imidazol-4-yl]methanol

生成物 1

HCID 545629854-Cyano-3-fluorophenyl 1-(triphenylmethyl)imidazol-4-yl ketone

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of (4-cyano-3-fluorophenyl)[1-(triphenylmethyl)imidazol-4-yl]methanol from Step D (10.0 g, 21.8 mmol) in CH2Cl2 (300 mL) was added MnO2 (18.9 g, 218 mmol) and the resulting mixture was heated to reflux for 18 hrs. The mixture was allowed to cool, then filtered through a pad of celite, washing with CH2Cl2. The filtrate was concentrated under reduced pressure to provide the titled product as a white solid that was sufficiently pure for use in the next step.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux for 18 hrs
  3. temperatureto cool
  4. filtrationfiltered through a pad of celite
  5. washwashing with CH2Cl2
  6. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-459d4844b59743eab0b9371f431ccad0
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06358985B1

反応ノート

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