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Tetrahydrofuran → 1-(2-Methylpyridin-4-yl)-5-(pyridin-2-ylmethylene)-5,7,8,9-tetrahydrocyclohepta[f]indazol

HRID 718823
ノート
印刷プレビュー

反応式

HRID 718823 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([N:8]2[C:16]3[C:11](=[CH:12][C:13]4[CH2:21][C:20](=O)[CH2:19][CH2:18][CH2:17][C:14]=4[CH:15]=3)[CH:10]=[N:9]2)[CH:5]=[CH:4][N:3]=1.C1COCC1.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[N:38]1[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=1[CH:44]=O>O>[CH3:1][C:2]1[CH:7]=[C:6]([N:8]2[C:16]3[C:11](=[CH:12][C:13]4[C:21](=[CH:44][C:39]5[CH:40]=[CH:41][CH:42]=[CH:43][N:38]=5)[CH2:20][CH2:19][CH2:18][CH2:17][C:14]=4[CH:15]=3)[CH:10]=[N:9]2)[CH:5]=[CH:4][N:3]=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 8028TetrahydrofuranHCID 142732-PyridinecarboxaldehydeHCID 2733832Lithium hexamethyldisilazaneHCID 867224321-(2-methylpyridin-4-yl)-5,7,8,9-tetrahydrocyclohepta[f]indazol-6(1H)-one

生成物 1

HCID 867224331-(2-Methylpyridin-4-yl)-5-(pyridin-2-ylmethylene)-5,7,8,9-tetrahydrocyclohepta[f]indazol

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
-77 °C

実験手順

A round bottom flask was charged with 1-(2-methylpyridin-4-yl)-5,7,8,9-tetrahydrocyclohepta[f]indazol-6(1H)-one (6, R1=2-methylpyridin-4-yl) (2.83 g, 9.71 mmol) and THF (43 mL). The solution was cooled to about −77° C. and then lithium bis(trimethylsilyl)amide (1.0 M in THF, 10.0 mL, 10.0 mmol) was added over about 30 min, keeping the internal temperature below about −75° C. After the addition was the mixture was stirred for about 5 min, the cold bath was removed and the mixture was allowed to warm to about 0° C. over about 1 h. The mixture was again cooled to about −75° C. then 2-pyridinecarboxaldehyde (3.2 mL, 34 mmol) was added. The mixture was allowed to warm to about −10° C. over about 1 h, and then water (40 mL) was added and the layers were separated. The aqueous layer was extracted with EtOAc (2×40 mL) and then the combined organics were washed with brine (50 mL), dried over Na2SO4 and then concentrated under reduced pressure. The crude material was purified on silica gel (120 g, eluted with 0% to 2.5% MeOH in DCM). Collection and concentration of the appropriate fractions gave 1-(2-methylpyridin-4-yl)-5-(pyridin-2-ylmethylene)-5,7,8,9-tetrahydrocyclohepta[f]indazol-6(1H-one (83, R1=2-methylpyridin-4-yl, R2′=pyridin-2-yl) (3.45 g, 93%) LC/MS, method 3, Rt=1.95 min, MS m/z 381 (M+H)+. 1H NMR (400 MHz, CDCl3) δ 8.65 (d, J=5.7 Hz, 1H), 8.61-8.53 (m, 1H), 8.11-8.08 (m, 1H), 7.95 (s, 1H), 7.82 (s, 1H), 7.80-7.64 (m, 2H), 7.53 (s, 1H), 7.44-7.35 (m, 1H), 7.14-7.06 (m, 1H), 6.92 (d, J=7.9 Hz, 1H), 3.14-3.06 (m, 2H), 2.78 (s, 3H), 2.56-2.48 (m, 2H), 2.23-2.08 (m, 2H).

後処理

  1. customthe internal temperature below about −75° C
  2. additionAfter the addition
  3. customthe cold bath was removed
  4. temperatureto warm to about 0° C. over about 1 h
  5. temperatureThe mixture was again cooled to about −75° C.
  6. temperatureto warm to about −10° C. over about 1 h
  7. customthe layers were separated
  8. extractionThe aqueous layer was extracted with EtOAc (2×40 mL)
  9. washthe combined organics were washed with brine (50 mL)
  10. dry with materialdried over Na2SO4
  11. concentrationconcentrated under reduced pressure
  12. customThe crude material was purified on silica gel (120 g, eluted with 0% to 2.5% MeOH in DCM)
  13. customCollection and concentration of the appropriate fractions

出典と根拠

ORDレコード
ord-37177e21982b4a31914f59e7962a6712
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09193744B2

反応ノート

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