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Hydrochloric Acid → [6-Hydroxy-2-(2,4,6-trifluoro-phenyl)-naphthalen-1-yl]-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methanone

HRID 1513926
ノート
印刷プレビュー

反応式

HRID 1513926 の反応式
C[O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([C:13]([C:15]1[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][N:24]3[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]3)=[CH:17][CH:16]=1)=[O:14])=[C:8]([C:30]1[C:35]([F:36])=[CH:34][C:33]([F:37])=[CH:32][C:31]=1[F:38])[CH:7]=[CH:6]2.Cl.C(OCC)C.B(Br)(Br)Br.C(=O)(O)[O-].[Na+]>ClCCl.CO>[OH:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([C:13]([C:15]1[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][N:24]3[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29]3)=[CH:17][CH:16]=1)=[O:14])=[C:8]([C:30]1[C:35]([F:36])=[CH:34][C:33]([F:37])=[CH:32][C:31]=1[F:38])[CH:7]=[CH:6]2
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

8

反応物 5

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 57552534[6-Methoxy-2-(2,4,6-trifluoro-phenyl)-naphthalen-1-yl]-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methanone

生成物 1

HCID 67004176
[6-Hydroxy-2-(2,4,6-trifluoro-phenyl)-naphthalen-1-yl]-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methanone
収率 87%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Alternatively, dissolve [6-methoxy-2-(2,4,6-trifluoro-phenyl)-naphthalen-1-yl]-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methanone (1.90 g, 3.67 mmol) in dichloromethane (10 ml). Add 2 M HCl in diethyl ether (4.0 mL, 80 mmol). Concentrate the slurry and dry in vacuo. Dilute the residue in dichloromethane (30 ml) and blanket with nitrogen. Cool the solution to 0° C. with an external ice bath. Add boron tribromide (1 mL, 11 mmol). After 60 minutes, pour the reaction mixture into a mixture of ice (20 g), methanol (10 mL) and saturated sodium bicarbonate solution (20 mL). Extract with dichloromethane (100 mL). Separate the layers, wash the organic layer with brine (20 mL), dry with magnesium sulfate, filter, and concentrate in vacuo. Purify the residue over silica gel, eluting the material with a step gradient of methanol/dichloromethane (0 to 10%), to give 1.6 g (87%) of the title compound: mass spectrum (ion spray) m/z=506.2 (M+H).

後処理

  1. concentrationConcentrate the slurry
  2. customdry in vacuo
  3. additionDilute the residue in dichloromethane (30 ml)
  4. additionpour the reaction mixture
  5. extractionExtract with dichloromethane (100 mL)
  6. customSeparate the layers
  7. washwash the organic layer with brine (20 mL)
  8. dry with materialdry with magnesium sulfate
  9. filtrationfilter
  10. concentrationconcentrate in vacuo
  11. customPurify the residue over silica gel
  12. washeluting the material with a step gradient of methanol/dichloromethane (0 to 10%)

出典と根拠

ORDレコード
ord-82f4eacc500944e3be5f6007ab38bfb6
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217032B2

反応ノート

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