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Carvacrol → 6-Chloro-4-isopropoxy-3-(5-isopropyl-2-methyl-phenoxymethyl)-2-methyl-pyridine

HRID 251647
ノート
印刷プレビュー

反応式

HRID 251647 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].C(O[C:11](=O)[C:12]1[C:17]([O:18][CH:19]([CH3:21])[CH3:20])=[CH:16][C:15]([Cl:22])=[N:14][C:13]=1[CH3:23])(C)C.O=S(Cl)Cl.C([O-])([O-])=O.[Cs+].[Cs+].[CH:35]1[C:42]([CH:43]([CH3:45])[CH3:44])=[CH:41][CH:40]=[C:38]([CH3:39])[C:36]=1[OH:37]>C1COCC1.C(Cl)Cl.O>[Cl:22][C:15]1[N:14]=[C:13]([CH3:23])[C:12]([CH2:11][O:37][C:36]2[CH:35]=[C:42]([CH:43]([CH3:45])[CH3:44])[CH:41]=[CH:40][C:38]=2[CH3:39])=[C:17]([O:18][CH:19]([CH3:21])[CH3:20])[CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 10364CarvacrolHCID 10796Cesium carbonateHCID 24386Thionyl ChlorideHCID 21226445Aluminium lithium hydrideHCID 865939896-Chloro-4-isopropoxy-2-methyl-nicotinic acid isopropyl ester

生成物 1

HCID 865939916-Chloro-4-isopropoxy-3-(5-isopropyl-2-methyl-phenoxymethyl)-2-methyl-pyridine

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

LiAlH4 (14 mL of 1 M solution in THF, 14 mmol) is added to a solution of 6-chloro-4-isopropoxy-2-methyl-nicotinic acid isopropyl ester (2.0 g, 7.4 mmol) in THF (10 mL) at 0° C. The mixture is stirred for 3 hours at ambient temperature. After quenching with water, the mixture is extracted with EtOAc. The combined extracts are washed with saturated brine, dried (Na2SO4), and concentrated to give the crude alcohol as a colorless oil which is dissolved in CH2Cl2 (10 mL) and treated with SOCl2 (2.7 mL, 37 mmol). The mixture is stirred for 1 hour at room temperature and concentrated in vacuo. The residue is dissolved in DMF (15 mL). To this is added Cs2CO3 (7.2 g, 11 mmol) and carvacrol (1.6 g, 11 mmol). The mixture is stirred for 16 hours at room temperature, poured into water, and extracted with Et2O. The combined extracts are washed with saturated brine, dried (Na2SO4), and concentrated in vacuo. The residue is purified by flash chromatography (elution with Hex/EtOAc 6:1) to yield 6-chloro-4-isopropoxy-3-(5-isopropyl-2-methyl-phenoxymethyl)-2-methyl-pyridine. 1H NMR (CDCl3) 7.05 (d, 1H), 6.82 (s, 1H), 6.79 (d, 1H), 6.724 (s, 1H), 5.02 (s, 2H), 4.60 (m, 1H), 2.88 (m, 1H), 2.59 (s, 3H), 2.12 (s, 3H), 1.37 (d, 6H), 1.24 (d, 6H).

後処理

  1. customAfter quenching with water
  2. extractionthe mixture is extracted with EtOAc
  3. washThe combined extracts are washed with saturated brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated
  6. customto give the crude alcohol as a colorless oil which
  7. stirringThe mixture is stirred for 1 hour at room temperature
  8. concentrationconcentrated in vacuo
  9. dissolutionThe residue is dissolved in DMF (15 mL)
  10. stirringThe mixture is stirred for 16 hours at room temperature
  11. extractionextracted with Et2O
  12. washThe combined extracts are washed with saturated brine
  13. dry with materialdried (Na2SO4)
  14. concentrationconcentrated in vacuo
  15. customThe residue is purified by flash chromatography (elution with Hex/EtOAc 6:1)

出典と根拠

ORDレコード
ord-f2eaa5e6db2c4375b85bf303909c4c20
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07863454B2

反応ノート

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