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1,2-Dichloroethane → HCID 178420189, 화합물

HRID 2303330
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HRID 2303330 반응식
[CH2:1]([CH:8]1[CH2:14][CH:13]2[NH:15][CH:10]([CH2:11][CH2:12]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH:16]1[CH:20]=[C:19]([CH2:21][CH2:22][CH:23]=[O:24])[N:18]=[CH:17]1.ClCCCl.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(Cl)(Cl)Cl.C([O-])([O-])=O.[Na+].[Na+]>[NH4+:15].[OH-:24].[CH2:1]([CH:8]1[CH2:14][CH:13]2[N:15]([CH2:23][CH2:22][CH2:21][C:19]3[N:18]=[CH:17][NH:16][CH:20]=3)[CH:10]([CH2:11][CH2:12]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 111,2-DichloroethaneHCID 5049666Sodium triacetoxyborohydrideHCID 18461105338733-58-7HCID 178520508HCID 178520508, 화합물

생성물 2

HCID 14923Ammonium HydroxideHCID 178420189HCID 178420189, 화합물수율 130.1%

시약·촉매·용매 2

HCID 6212
Chloroform
용매
HCID 10340Sodium Carbonate용매

실험 절차

A mixture of 0.25 g of 3-benzyl-8-aza-bicyclo[3.2.1]octane, 0.45 g of 3-(1H-imidazol-4-yl)-propionaldehyde, 5 mL of 1,2-dichloroethane and 0.5 g of sodium triacetoxyborohydride was stirred at room temperature for 48 h. The reaction mixture was diluted with 50 mL chloroform and 10 mL saturated aqueous Na2CO3 and the layers separated. The aqueous layer was extracted with 2×25 mL of chloroform and the combined organic layers dried over magnesium sulfate and concentrated under reduced pressure. Purification by chromatography eluting with 90:10:1 CHCl3:MeOH:NH4OH gave 0.25 g of 3-benzyl-8-[3-(1H-imidazol-4-yl)-propyl]-8-aza-bicyclo[3.2.1]octane as a 2:1 mixture of exo:endo isomers. MS (m+1)=310.3; 1H NMR (400 MHz, CDCl3) 7.5-7.1 (complex, 6H), 6.75 (s, 1H), 3.22 (s, 2H), 2.75 (m, 2.6 H), 2.5 (d, 0.7×2H), 2.45 (m, 2H), 2.1 (m, 2H), 1.95 (m, 2H), 1.8 (m, 3H), 1.5 (m, 4H).

후처리

  1. customthe layers separated
  2. extractionThe aqueous layer was extracted with 2×25 mL of chloroform
  3. dry with materialthe combined organic layers dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customPurification by chromatography
  6. washeluting with 90:10:1 CHCl3

출처 및 근거

ORD 기록
ord-803556e40d5647d1820ec53668b0388a
출처 데이터셋
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06432976B1

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