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Isopropyl iodide → 3-Methyl-1-(1-methylethyl)-4-({1-[3-(trifluoromethyl)phenyl]-1H-tetrazol-5-yl}methyl)-2-piperazinone

HRID 517769
ノート
印刷プレビュー

反応式

HRID 517769 の反応式
[CH3:1][CH:2]1[N:7]([CH2:8][C:9]2[N:13]([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=3)[N:12]=[N:11][N:10]=2)[CH2:6][CH2:5][NH:4][C:3]1=[O:24].I[CH:26]([CH3:28])[CH3:27].[H-].[Na+]>CN(C)C=O.C(OCC)(=O)C>[CH3:1][CH:2]1[N:7]([CH2:8][C:9]2[N:13]([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=3)[N:12]=[N:11][N:10]=2)[CH2:6][CH2:5][N:4]([CH:26]([CH3:28])[CH3:27])[C:3]1=[O:24]
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 6362Isopropyl iodide2 回HCID 24758Sodium hydride2 回HCID 566001413-Methyl-4-({1-[3-(trifluoromethyl)phenyl]-1H-tetrazol-5-yl}methyl)-2-piperazinone2 回

生成物 1

HCID 566001393-Methyl-1-(1-methylethyl)-4-({1-[3-(trifluoromethyl)phenyl]-1H-tetrazol-5-yl}methyl)-2-piperazinone収率 9.5%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 3-methyl-4-({1-[3-(trifluoromethyl)phenyl]-1H-tetrazol-5-yl}methyl)-2-piperazinone (75 mg, 0.220 mmol, Compound 32), in N,N-Dimethylformamide (DMF) (1 mL) was added 2-iodopropane (0.024 mL, 0.242 mmol) and sodium hydride (8.81 mg, 0.220 mmol). The resulting reaction mixture was stirred at room temperature for 24 hours. To the reaction mixture was added 1 equivalent of 2-iodopropane and 0.5 equivalent of sodium hydride and stirred for an additional 24 h at room temperature. The reaction mixture was diluted with ethyl acetate (20 mL) and washed with 2N NaOH solution (10 mL). The aqueous phase was extracted with ethyl acetate (2×10 mL). All of the organic phases were combined, dried over magnesium sulphate, filtered and concentrated. The crude product was purified by MDAP. The relevant fractions were combined, concentrated and dried to give the title compound as a colourless oil (8 mg).

後処理

  1. customThe resulting reaction mixture
  2. stirringstirred for an additional 24 h at room temperature
  3. washwashed with 2N NaOH solution (10 mL)
  4. extractionThe aqueous phase was extracted with ethyl acetate (2×10 mL)
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude product was purified by MDAP
  9. concentrationconcentrated
  10. customdried

出典と根拠

ORDレコード
ord-f6ba4a87b1424f01ac51c6c7eb494db7
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115132B2

反応ノート

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