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Hydrochloric Acid → 2-(tert-Butyl-dimethyl-silanyloxy)-5-{2-[4-(2-chloro-ethoxy)-phenyl]-7-methoxy-4-methyl-2H-chromen-3-yl}-pyridine

HRID 747875
ノート
印刷プレビュー

反応式

HRID 747875 の反応式
[Cl:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8](I)=[CH:7][CH:6]=1.[Li]CCCC.[C:17]([Si:21]([CH3:44])([CH3:43])[O:22][C:23]1[N:28]=[CH:27][C:26]([C:29]2[CH:30](O)[O:31][C:32]3[C:37]([C:38]=2[CH3:39])=[CH:36][CH:35]=[C:34]([O:40][CH3:41])[CH:33]=3)=[CH:25][CH:24]=1)([CH3:20])([CH3:19])[CH3:18].Cl>O1CCCC1.C1(C)C=CC=CC=1.CCCCCC>[C:17]([Si:21]([CH3:44])([CH3:43])[O:22][C:23]1[CH:24]=[CH:25][C:26]([C:29]2[CH:30]([C:8]3[CH:9]=[CH:10][C:5]([O:4][CH2:3][CH2:2][Cl:1])=[CH:6][CH:7]=3)[O:31][C:32]3[C:37]([C:38]=2[CH3:39])=[CH:36][CH:35]=[C:34]([O:40][CH3:41])[CH:33]=3)=[CH:27][N:28]=1)([CH3:20])([CH3:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 113580261-(2-Chloroethoxy)-4-iodobenzeneHCID 115168783-[6-(tert-butyl-dimethyl-silanyloxy)-pyridin-3-yl]-7-methoxy-4-methyl-2H-chromen-2-olHCID 178418339Butyllithium

生成物 1

HCID 114975112-(tert-Butyl-dimethyl-silanyloxy)-5-{2-[4-(2-chloro-ethoxy)-phenyl]-7-methoxy-4-methyl-2H-chromen-3-yl}-pyridine

試薬・触媒・溶媒 3

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒

実験手順

In a single neck, 100 mL round bottom flask was dissolved and stirred 1-(2-chloro-ethoxy)-4-iodo-benzene (530 mg, 1.88 mmol, 5.0 eq), in tetrahydrofuran (5 mL) under nitrogen, and the mixture cooled to −78° C. After 5 minutes of stirring, a hexane solution of n-BuLi (0.75 mL of 2.5 M, 1.88 mmol, 5.0 eq) was added via syringe. The reaction mixture was then stirred for 30 min at about −78° C. A tetrahydrofuran solution of 3-[6-(tert-butyl-dimethyl-silanyloxy)-pyridin-3-yl]-7-methoxy-4-methyl-2H-chromen-2-ol (150 mg, 0.376 mmol, 1 eq, in 2 mL), prepared as in Example 24, was then added, the cooling bath was removed and the reaction mixture was allowed to warm to room temperature overnight. After about 18 hours, the reaction was worked-up with addition of saturated ammonium acetate solution and extraction with ethyl ether. The combined organic extracts were washed with brine and water, dried with anhydrous sodium sulphate, filtered and evaporated to yield a sticky semisolid residue. To this solid was added 0.2 mL HCl in 10 mL toluene at room temperature. The mixture was stirred for 2 hours at room temperature. The reaction was worked-up with sodium bicarbonate washing and extraction with ethyl acetate three times. The combined organic extracts were washed with brine and water, dried with anhydrous sodium sulphate, filtered and evaporated to yield a brown oil. The title product was isolated as a white semisolid foam via chromatography on silica gel eluted with 1:1 hexanes:ethyl acetate as eluent.

後処理

  1. dissolutionIn a single neck, 100 mL round bottom flask was dissolved
  2. stirringThe reaction mixture was then stirred for 30 min at about −78° C
  3. additionwas then added
  4. customthe cooling bath was removed
  5. waitAfter about 18 hours
  6. additionthe reaction was worked-up with addition of saturated ammonium acetate solution and extraction with ethyl ether
  7. washThe combined organic extracts were washed with brine and water
  8. dry with materialdried with anhydrous sodium sulphate
  9. filtrationfiltered
  10. customevaporated
  11. customto yield a sticky semisolid residue
  12. stirringThe mixture was stirred for 2 hours at room temperature
  13. extractionThe reaction was worked-up with sodium bicarbonate washing and extraction with ethyl acetate three times
  14. washThe combined organic extracts were washed with brine and water
  15. dry with materialdried with anhydrous sodium sulphate
  16. filtrationfiltered
  17. customevaporated
  18. customto yield a brown oil

出典と根拠

ORDレコード
ord-66139a01bf5f4032bdea61237d4d5e97
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399767B2

反応ノート

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