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2,3-Dihydro-1,4-benzothiazine → N-{[2-(2,3-dihydro-4H-1,4-benzothiazin-4-yl)pyridine-3-yl]methyl}-N-pyridin-3-ylpyridin-3-amine

HRID 563948
ノート
印刷プレビュー

反応式

HRID 563948 の反応式
Cl[C:2]1[C:7]([CH2:8][N:9]([C:16]2[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=2)[C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.[S:22]1[C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=2[NH:25][CH2:24][CH2:23]1.CC(C)([O-])C.[Na+]>O1CCOCC1.C(Cl)Cl.[Pd].C(P(C(C)(C)C)C(C)(C)C)(C)(C)C.C(P(C(C)(C)C)C(C)(C)C)(C)(C)C>[S:22]1[C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=2[N:25]([C:2]2[C:7]([CH2:8][N:9]([C:16]3[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=3)[C:10]3[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=3)=[CH:6][CH:5]=[CH:4][N:3]=2)[CH2:24][CH2:23]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 1510642,3-Dihydro-1,4-benzothiazineHCID 23676156Sodium t-butoxideHCID 59138879N-[(2-chloropyridin-3-yl)methyl]-N-pyridin-3-ylpyridin-3-amine

生成物 1

HCID 24877535N-{[2-(2,3-dihydro-4H-1,4-benzothiazin-4-yl)pyridine-3-yl]methyl}-N-pyridin-3-ylpyridin-3-amine収率 75%

試薬・触媒・溶媒 3

HCID 2734558
Bis(tri-tert-butylphosphine)palladium(0)
触媒
HCID 6344Dichloromethane溶媒
HCID 312751,4-Dioxane溶媒

実験手順

To a solution of N-[(2-chloropyridin-3-yl)methyl]-N-pyridin-3-ylpyridin-3-amine (110 mg, 0.37 mmol) and 3,4-dihydro-2H-1,4-benzothiazine (85 mg, 0.56 mmol) (prepared according to procedure described in patent WO 0220498) in dry dioxane (1.25 mnL) was added sodium t-butoxide (48 mg, 0.50 mmol), and bis(tri-t-butylphosphine) palladium(0) (34 mg, 0.066 mmol). The vessel was sealed with a septum cap, degassed (3×), and heated at 100 C for 3 hours. The cooled reaction was diluted with methylene chloride and washed with NaHCO3 solution, and water and the organic layer was dried over anhydrous sodium sulfate, filtered, and the solvent evaporated. The residue was subjected to silica gel chromatography eluting with a 20-90% acetone/hexane gradient to give the title compound as a colorless glass(114 mg, 75% yield). 1H-NMR (500 MHz, CDCl3): δ 8.41 (1H, d, J=4.9 Hz), 8.28 (2H, d, J=3.7 Hz), 8.23 (2H, d, J=4.6 Hz), 7.70 (1H, d, J=6.1 Hz), 7.21-7.26 (4H, m), 7.17 (1H, d, J=3.7 Hz), 7.16 (1H, d, J=4.6 Hz), 7.06 (1H, dd, J=4.9, 7.6 Hz), 6.91 (1H, t, J=7.8 Hz), 6.84 (1H, t, J=7.6 Hz), 6.32 (1H, d, J=8.0 Hz), 4.56 (2H,s), 4.13 (2H, br s), 3.32 (2H, t, J=5.6 Hz). m/e (m+1): 412.2.

後処理

  1. customThe vessel was sealed with a septum
  2. customcap
  3. customdegassed (3×)
  4. temperatureheated at 100 C for 3 hours
  5. customThe cooled reaction
  6. washwashed with NaHCO3 solution, and water
  7. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. customthe solvent evaporated
  10. washeluting with a 20-90% acetone/hexane gradient

出典と根拠

ORDレコード
ord-2a45e8208eea4da6acc20370d7b5e6f7
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08067607B2

反応ノート

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