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(1,3,5-trimethyl-1H-pyrazol-4-yl)methylamine → [4-(2-o-Tolyl-chroman-6-yloxy)-cyclohexyl]-(1,3,5-trimethyl-1H-pyrazol-4-ylmethyl)-amine

HRID 59774
ノート
印刷プレビュー

反応式

HRID 59774 の反応式
[C:1]1([CH3:25])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]1[CH2:16][CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:17][CH:18]3[CH2:23][CH2:22][C:21](=O)[CH2:20][CH2:19]3)[CH:13]=2)[O:8]1.[CH3:26][N:27]1[C:31]([CH3:32])=[C:30]([CH2:33][NH2:34])[C:29]([CH3:35])=[N:28]1.C([BH3-])#N.[Na+]>CO.C(O)(=O)C>[C:1]1([CH3:25])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]1[CH2:16][CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:17][CH:18]3[CH2:23][CH2:22][CH:21]([NH:34][CH2:33][C:30]4[C:29]([CH3:35])=[N:28][N:27]([CH3:26])[C:31]=4[CH3:32])[CH2:20][CH2:19]3)[CH:13]=2)[O:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 2776430(1,3,5-trimethyl-1H-pyrazol-4-yl)methylamineHCID 5003444Sodium cyanoborohydrideHCID 90389985HCID 90389985、化合物

生成物 1

HCID 90390297[4-(2-o-Tolyl-chroman-6-yloxy)-cyclohexyl]-(1,3,5-trimethyl-1H-pyrazol-4-ylmethyl)-amine収率 95.7%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 887
Methanol
溶媒

実験手順

To a solution of 100 mg 4-(2-o-tolyl-chroman-6-yloxy)-cyclohexanone (0.30 mmol) in 2 ml of methanol and 0.15 ml of acetic acid at room temperature 124 mg (1,3,5-trimethyl-1H-pyrazol-4-yl-methyl)amine (0.89 mmol) and 56 mg of sodium cyanoborohydride (0.89 mmol) were added in one portion and stirring at room temperature was continued for 2 h. Volatile components were removed under reduced pressure and the resulting residue dissolved in dichloromethane. The organic layer was washed with aqueous 2N sodium hydroxide solution and saturated aqueous sodium chloride solution. The organic layer was dried with sodium sulfate and filtered, and the solvent removed under reduced pressure. The crude product was purified by reversed phase HPLC. 132 mg of the title compound were isolated.

後処理

  1. customVolatile components were removed under reduced pressure
  2. dissolutionthe resulting residue dissolved in dichloromethane
  3. washThe organic layer was washed with aqueous 2N sodium hydroxide solution and saturated aqueous sodium chloride solution
  4. dry with materialThe organic layer was dried with sodium sulfate
  5. filtrationfiltered
  6. customthe solvent removed under reduced pressure
  7. customThe crude product was purified by reversed phase HPLC

出典と根拠

ORDレコード
ord-bc102e7b04324135b795bff309f724c0
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09440941B2

反応ノート

読み込み中…

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