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Hydrochloric Acid → 4-(4-Bromo-2-methyl-phenyl)-1-methyl-3-(2-pyridyl)-4,6,7,8-tetrahydropyrazolo[3,4-e][1,4]thiazepine

HRID 1748796
ノート
印刷プレビュー

反応式

HRID 1748796 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[S:14][CH2:13][C:12](=O)[NH:11][C:10]3[N:16]([CH3:25])[N:17]=[C:18]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=4)[C:9]2=3)=[C:4]([CH3:26])[CH:3]=1.B.C1COCC1.Cl.[OH-].[Na+]>C1COCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[S:14][CH2:13][CH2:12][NH:11][C:10]3[N:16]([CH3:25])[N:17]=[C:18]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=4)[C:9]2=3)=[C:4]([CH3:26])[CH:3]=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 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 2723981Borane;tetrahydrofuranHCID 1363484514-(4-Bromo-2-methyl-phenyl)-1-methyl-3-(2-pyridyl)-4,8-dihydropyrazolo[3,4-e][1,4]thiazepin-7-one

生成物 1

HCID 1363484254-(4-Bromo-2-methyl-phenyl)-1-methyl-3-(2-pyridyl)-4,6,7,8-tetrahydropyrazolo[3,4-e][1,4]thiazepine収率 74%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-(4-bromo-2-methyl-phenyl)-1-methyl-3-(2-pyridyl)-4,8-dihydropyrazolo[3,4-e][1,4]thiazepin-7-one (2.92 g, 6.8 mmol) in anhydrous THF (50 mL) was added a solution of borane THF complex (27.2 mL, 1M in THF, 27.2 mmol, Acros) at about 0° C. Subsequently, the mixture was stirred at rt, overnight. After cooling to about 0° C., HCl (5 M aq, 20 mL) was added dropwise and the mixture was stirred for about 30 min at rt, then the solution was brought to about pH=7 with 2 M aq NaOH, at about 0° C. The resulting mixture was extracted with ethyl acetate (200 mL). The organic layer was washed with brine (50 mL), dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (SiO2, ethyl acetate) to give 4-(4-bromo-2-methyl-phenyl)-1-methyl-3-(2-pyridyl)-4,6,7,8-tetrahydropyrazolo[3,4-e]-[1,4]thiazepine (2.1 g, 5.0 mmol, 74%) as an off white solid: LC-MS (Table 1, Method e) Rt=8.32 min, m/z 415 (M+H)+; 1H-NMR (CDCl3, Bruker 400 MHz) δ 2.58 (3H, s) 2.69 (1H, ddd, J=15.0, 6.0, 2.0 Hz) 2.86 (1H, ddd, J=15.0, 9.0, 2.5 Hz) 3.21-3.31 (1H, m) 3.57-3.65 (1H, m) 3.79 (1H, br s) 3.83 (3H, s) 6.65 (1H, s) 7.04-7.09 (2H, m) 7.14 (1H, dd, J=8.5, 2.0 Hz) 7.31 (1H, d, J=2.0 Hz) 7.59 (1H, td, J=7.5, 2.0 Hz) 7.80 (1H, br.d, J=8.0 Hz) 8.45 (1H, br.d, J=5.0 Hz).

後処理

  1. temperatureAfter cooling to about 0° C.
  2. stirringthe mixture was stirred for about 30 min at rt
  3. extractionThe resulting mixture was extracted with ethyl acetate (200 mL)
  4. washThe organic layer was washed with brine (50 mL)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by column chromatography (SiO2, ethyl acetate)

出典と根拠

ORDレコード
ord-8487d251fad64ed39a034cc2cde33126
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150592B2

反応ノート

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