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Cyclohexylamine → HCID 58999039、化合物

HRID 2105781
ノート
印刷プレビュー

反応式

HRID 2105781 の反応式
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C[Al](C)C.C[O:13][C:14]([C:16]1[C:20]([CH3:21])=[C:19]([C:22]2[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:25]=[C:24]([C:32]([F:35])([F:34])[F:33])[CH:23]=2)[N:18]([CH2:36][CH:37]2[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]2)[C:17]=1[CH3:43])=O>C1(C)C=CC=CC=1>[CH:1]1([NH:7][C:14]([C:16]2[C:20]([CH3:21])=[C:19]([C:22]3[CH:27]=[C:26]([C:28]([F:29])([F:30])[F:31])[CH:25]=[C:24]([C:32]([F:35])([F:34])[F:33])[CH:23]=3)[N:18]([CH2:36][CH:37]3[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42]3)[C:17]=2[CH3:43])=[O:13])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7965CyclohexylamineHCID 16682925TrimethylaluminumHCID 86594074HCID 86594074、化合物

生成物 1

HCID 58999039HCID 58999039、化合物収率 50.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

実験手順

A solution of 59.5 μl (0.52 mmol) of cyclohexylamine in toluene (2 ml) was treated at RT dropwise with 0.26 μl of a 2 M solution of trimethylaluminum in toluene (0.52 mmol). The reaction solution was stirred 1 h at RT, 200 mg (0.43 mmol) of 5-(3,5-bis-trifluoromethyl-phenyl)-1-cyclohexylmethyl-2,4-dimethyl-1H-pyrrole-3-carboxylic acid methyl ester in toluene (2 ml) were added and reaction mixture was heated at 110° C. for 3 h. The mixture was then partitioned between water and ethyl acetate, the organic layer was isolated, dried over sodium sulfate and concentrated in vacuo and purified by column chromatography to give 114 mg of the title compound, MS (ISP) 529.3 (M+H)+.

後処理

  1. customreaction mixture
  2. temperaturewas heated at 110° C. for 3 h
  3. customThe mixture was then partitioned between water and ethyl acetate
  4. customthe organic layer was isolated
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. custompurified by column chromatography

出典と根拠

ORDレコード
ord-13fa80e50bfa4dc2a65574192d2ada59
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07579369B2

反応ノート

読み込み中…

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