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Dimethylformamide dimethyl acetal → 4-[5-(2-Methylthiopyrimidin-4-yl)-1-methyl-4-(3-trifluoromethylphenyl)-1H-imidazol-2-yl]-piperidine-1-carboxylic acid benzyl ester

HRID 342693
ノート
印刷プレビュー

反応式

HRID 342693 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([C:17]2[NH:18][C:19]([C:32]3[CH:37]=[CH:36][N:35]=[C:34]([S:38][CH3:39])[N:33]=3)=[C:20]([C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=3)[N:21]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:40]OC(OC)N(C)C>C1(C)C=CC=CC=1>[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([C:17]2[N:18]([CH3:40])[C:19]([C:32]3[CH:37]=[CH:36][N:35]=[C:34]([S:38][CH3:39])[N:33]=3)=[C:20]([C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:29])([F:31])[F:30])[CH:23]=3)[N:21]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 2

HCID 78373Dimethylformamide dimethyl acetalHCID 106503634-[5-(2-Methylthiopyrimidin-4-yl)-4-(3-trifluoromethylphenyl)-1H-imidazol-2-yl]piperidine-1-carboxylic acid benzyl ester

生成物 1

HCID 106030804-[5-(2-Methylthiopyrimidin-4-yl)-1-methyl-4-(3-trifluoromethylphenyl)-1H-imidazol-2-yl]-piperidine-1-carboxylic acid benzyl ester

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirring solution of 4-[5-(2-methylthiopyrimidin-4-yl)-4-(3-trifluoromethylphenyl)-1H-imidazol-2-yl]-piperidine-1-carboxylic acid benzyl ester (Example 1E) (4.0 g, 7.22 mmole) in toluene (80 mL) was added dimethylformamide dimethyl acetal (4.0 mL) and the mixture heated to reflux for 18 hours. The reaction was cooled, concentrated in vacuo to a foam and chromatographed on silica using 5% acetone/methylene chloride to give upon concentration of the product containing fractions the title compound 2.78 g.

後処理

  1. temperaturethe mixture heated
  2. temperatureto reflux for 18 hours
  3. temperatureThe reaction was cooled
  4. concentrationconcentrated in vacuo to a foam
  5. customchromatographed on silica using 5% acetone/methylene chloride
  6. customto give upon concentration of the product

出典と根拠

ORDレコード
ord-e0bf5bcc26c744469a59c761258c447c
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05859041

反応ノート

読み込み中…

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