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Dimethylformamide → HCID 58968646、化合物

HRID 2075042
ノート
印刷プレビュー

反応式

HRID 2075042 の反応式
[Br:1][C:2]1[CH:29]=[C:28]([CH3:30])[C:27]([C:31]([F:34])([F:33])[F:32])=[CH:26][C:3]=1[CH2:4][N:5]([CH2:11][C:12]1[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[C:14]([C:22]([F:25])([F:24])[F:23])[CH:13]=1)[C:6]1[N:7]=[N:8][NH:9][N:10]=1.[C:35](=O)([O-])[O-].[Na+].[Na+].CN(C)C=O.S(OC)(OC)(=O)=O>C1COCC1>[Br:1][C:2]1[CH:29]=[C:28]([CH3:30])[C:27]([C:31]([F:34])([F:32])[F:33])=[CH:26][C:3]=1[CH2:4][N:5]([CH2:11][C:12]1[CH:13]=[C:14]([C:22]([F:23])([F:24])[F:25])[CH:15]=[C:16]([C:18]([F:19])([F:20])[F:21])[CH:17]=1)[C:6]1[N:7]=[N:8][N:9]([CH3:35])[N:10]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6497Dimethyl SulfateHCID 10340Sodium CarbonateHCID 58968655N-(2-bromo-4-methyl-5-(trifluoromethyl)benzyl)-N-(3,5-bis(trifluoromethyl)benzyl)-2H-tetrazol-5-amine

生成物 1

HCID 58968646HCID 58968646、化合物収率 97.7%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
70 °C

実験手順

To a solution of N-(2-bromo-4-methyl-5-(trifluoromethyl)benzyl)-N-(3,5-bis(trifluoromethyl)benzyl)-2H-tetrazol-5-amine (76 mg, 0.135 mmol) in anhydrous THF (5 mL) was added sodium carbonate (28 mg, 0.270 mmol) and N,N-dimethylformamide (1 mL) followed by dimethyl sulfate (34 mg. 0.270 mmol). The solution was heated to 70° C. for 18 hours then the solvent was removed under reduced pressure. The residue was partitioned between ethyl acetate (20 mL) and water (10 mL). The aqueous layer was extracted with ethyl acetate (3×20 mL) and the combined organics were washed with water (3×20 mL). The combined organics were dried with anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give the title compound (76 mg, 97.5%). 1H NMR (400 MHz, CDCl3) δ 7.71 (s, 1H) 7.62 (s, 2H) 7.44(s, 1H) 7.40(s, 1H) 4.79(s, 2H) 4.76(s, 2H) 4.20(s, 3H) 2.39(s, 3H). LC-MS calc. 576 found 577 (M+H)

後処理

  1. customthe solvent was removed under reduced pressure
  2. customThe residue was partitioned between ethyl acetate (20 mL) and water (10 mL)
  3. extractionThe aqueous layer was extracted with ethyl acetate (3×20 mL)
  4. washthe combined organics were washed with water (3×20 mL)
  5. dry with materialThe combined organics were dried with anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-175c826b8b68407681bf5baab886e087
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07919506B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート