Ethyl Acetate → HCID 86657565、化合物

HRID 38722

反応式

HRID 38722 の反応式
C(N[C:5]1[CH:10]=[CH:9][C:8](S(N=[N+]=[N-])(=O)=O)=[CH:7][CH:6]=1)(=O)C.O=[C:18](C)[CH2:19]P(=O)(OC)OC.[F:27][CH:28]([F:64])[C:29]1[CH:33]=[C:32]([CH:34]([F:36])[F:35])[N:31]([CH2:37][C:38]([N:40]2[CH2:45][CH2:44][CH:43]([C:46]3[S:47][CH:48]=[C:49]([C:51]4[CH2:55][CH:54](C5C=CC=CC=5C=O)[O:53][N:52]=4)[N:50]=3)[CH2:42][CH2:41]2)=[O:39])[N:30]=1.C(OCC)(=O)C>C(#N)C.CO.O>[F:64][CH:28]([F:27])[C:29]1[CH:33]=[C:32]([CH:34]([F:36])[F:35])[N:31]([CH2:37][C:38]([N:40]2[CH2:45][CH2:44][CH:43]([C:46]3[S:47][CH:48]=[C:49]([C:51]4[CH2:55][CH:54]([C:5]5[CH:6]=[CH:7][CH:8]=[CH:9][C:10]=5[C:18]#[CH:19])[O:53][N:52]=4)[N:50]=3)[CH2:42][CH2:41]2)=[O:39])[N:30]=1

参加物

8

反応物 4

HCID 8857Ethyl AcetateHCID 77872Dimethyl (2-oxopropyl)phosphonateHCID 51291854-Acetamidobenzenesulfonyl azideHCID 86657566HCID 86657566、化合物

生成物 1

HCID 86657565HCID 86657565、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

To a solution of 4-acetamidobenzenesulphonyl azide (140 mg) in acetonitrile (10 ml) was added, at room temperature, dimethyl 2-oxopropylphosphonate (97 mg). After stirring for 2 hours, 2-{3-[2-(1-{[3,5-bis(difluoromethyl)-1H-pyrazol-1-yl]acetyl}piperidin-4-yl)-1,3-thiazol-4-yl]-4,5-dihydro-1,2-oxazol-5-yl}benzaldehyde (267 mg) in methanol (2 ml) was added to the reaction mixture. After stirring for 8 hours, the reaction mixture was admixed with ethyl acetate and water and extracted with ethyl acetate. The organic extracts were dried over sodium sulphate and concentrated under reduced pressure. The residue was purified by chromatography. This gave tert-2-[3,5-bis(difluoromethyl)-1H-pyrazol-1-yl]-1-(4-{4-[5-(2-ethynylphenyl)-4,5-dihydro-1,2-oxazol-3-yl]-1,3-thiazol-2-yl}piperidin-1-yl)ethanone (50 mg).

後処理

  1. stirringAfter stirring for 8 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic extracts were dried over sodium sulphate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by chromatography

出典と根拠

ORDレコード
ord-46d18b2aeb4b45df8b337b9f435ebe4d
出典データセット
uspto-grants-2013_09
特許番号
US08524743B2

関連ノート

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