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9-Fluorenylmethyl chloroformate → HCID 22872534, 화합물

HRID 1779970
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HRID 1779970 반응식
COC1[C@@H](C(C)C)N=[C:6]([O:12][CH3:13])[C@H:7]([CH2:9][O:10][CH3:11])[N:8]=1.[C:17](Cl)([O:19][CH2:20][CH:21]1[C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:27]2[C:22]1=[CH:23][CH:24]=[CH:25][CH:26]=2)=[O:18].C([O-])(O)=[O:36].[Na+]>O1CCOCC1.O.C(Cl)(Cl)Cl>[CH:32]1[C:33]2[CH:21]([CH2:20][O:19][C:17]([NH:8][C@@H:7]([CH2:9][O:10][CH3:11])[C:6]([O:12][CH3:13])=[O:36])=[O:18])[C:22]3[C:27](=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:28]=2[CH:29]=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 343679-Fluorenylmethyl chloroformateHCID 516892Sodium BicarbonateHCID 57294432HCID 57294432, 화합물

생성물 1

HCID 22872534HCID 22872534, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6212Chloroform용매
HCID 31275
1,4-Dioxane
용매
2회

실험 절차

To a solution of (2R,5S)-3,6-dimethoxy-5-(methoxymethyl)-2-isopropyl-2,5-dihydropyrazine (2.1 g, 9.2 mmol) in dioxane (18 ml ) 1M HCl (18.4 ml ), 18.4 mmol) was added and the mixture stirred at ambient temperature overnight. The volatile components were evaporated, the residue redissolved in dioxane and again evaporated. The crude residue was dissolved dioxane and FmocCl (5.71 g, 2.21 mmol) was added. After 2 minutes 1M NaHCO3 (44.2 ml, 44.2 mmol) was added. After 15 minutes the mixture was diluted with water (50 ml) and CHCl3 (100 ml). The layers were separated and the aqueous phase extracted with CHCl3 (2×75 ml). The combined organic layer was dried (Na2SO4), concentrated and purified by flash chromatography (silica gel; hexane: ethyl acetate 2:1).

후처리

  1. customThe volatile components were evaporated
  2. dissolutionthe residue redissolved in dioxane
  3. customagain evaporated
  4. additionwas added
  5. customThe layers were separated
  6. extractionthe aqueous phase extracted with CHCl3 (2×75 ml)
  7. dry with materialThe combined organic layer was dried (Na2SO4)
  8. concentrationconcentrated
  9. custompurified by flash chromatography (silica gel; hexane: ethyl acetate 2:1)

출처 및 근거

ORD 기록
ord-5073e6f75b62487185cd8679160e8b71
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05629293

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