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Chloroacetyl chloride → HCID 69701133, 화합물

HRID 1596091
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HRID 1596091 반응식
C1(C)C=CC(S(Cl)(=O)=O)=CC=1.[Cl:12][C:13]1[CH:14]=[C:15]([CH:20](O)[C@H:21]([OH:44])[CH2:22][CH2:23][O:24][C:25]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:16]=[CH:17][C:18]=1[Cl:19].O.O.O.Cl([O-])(=O)(=O)=O.[Li+].[CH:55]1([CH2:61][NH2:62])[CH2:60][CH2:59][CH2:58][CH2:57][CH2:56]1.C(N(CC)CC)C.[Cl:70][CH2:71][C:72](Cl)=[O:73]>N1C=CC=CC=1.C(Cl)Cl.C(OCC)(=O)C.O>[C:38]1([C:25]([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[O:24][CH2:23][CH2:22][C@@H:21]([OH:44])[CH:20]([C:15]2[CH:16]=[CH:17][C:18]([Cl:19])=[C:13]([Cl:12])[CH:14]=2)[N:62]([C:72](=[O:73])[CH2:71][Cl:70])[CH2:61][CH:55]2[CH2:60][CH2:59][CH2:58][CH2:57][CH2:56]2)[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 6

HCID 6577Chloroacetyl chlorideHCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 76688CyclohexanemethylamineHCID 23708903Lithium perchlorate trihydrateHCID 53669173HCID 53669173, 화합물

생성물 1

HCID 69701133
HCID 69701133, 화합물
수율 63%

시약·촉매·용매 4

HCID 962Water용매HCID 1049Pyridine용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

p-Toluenesulfonyl chloride (2.03g, 10.7 mmol) was added to a solution of (2R)-(3,4-dichlorophenyl)-4-(triphenylmethoxy)butan-1,2-diol (3.51 g, 7.11 mmol), which was prepared in Example 12(a), in pyridine (17 ml). The mixture was stirred at room temperature overnight. To the reaction mixture, water was added and it was extracted with ethyl acetate. The organic layer was dried over anydrous magnesium sulfate and then the solvent was distilled off under reduced pressure. The residue was dissolved in acetonitrile (50 ml) and lithium perchlorate trihydrate (3.42 g. 21.3 mmol) and cyclohexylmethylamine (2.78 ml, 21.3 mmol) were added to the solution. The mixture was stirred at 100° C. overnight. Ethyl acetate was added to the reaction mixture and it was washed with a saturated aqueous solution of sodium chloride. The organic layer was dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure. A half of the residue by weight was dissolved in methylene chloride (30 ml). To this solution, triethylamine (2.48 ml, 17.8 mmol) and chloroacetyl chloride (1.42 ml, 17.8 mmol) were added with ice-cooling. The mixture was stirred at 0° C. for 1 hour. To the reaction mixture, methylene chloride was added, the organic layer was washed with water and then with a saturated aquoeus solution of sodium chloride and was dried over anhydrous magnesium sulfate. After distillation under reduced pressure, the resulting residue was purified by flash chromatography on a silica gel column using n-hexane/ethyl acetate=20/1−10/1 as an eluant to afford the title compound (1.49 g, 63%).

후처리

  1. extractionit was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. dissolutionThe residue was dissolved in acetonitrile (50 ml)
  5. stirringThe mixture was stirred at 100° C. overnight
  6. washwas washed with a saturated aqueous solution of sodium chloride
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. dissolutionA half of the residue by weight was dissolved in methylene chloride (30 ml)
  10. temperaturecooling
  11. stirringThe mixture was stirred at 0° C. for 1 hour
  12. washthe organic layer was washed with water
  13. dry with materialwith a saturated aquoeus solution of sodium chloride and was dried over anhydrous magnesium sulfate
  14. distillationAfter distillation under reduced pressure
  15. customthe resulting residue was purified by flash chromatography on a silica gel column

출처 및 근거

ORD 기록
ord-923e8a331ff8427a91628567e3f39522
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06288059B1

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