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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → HCID 70270103, 화합물

HRID 2292993
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HRID 2292993 반응식
[CH3:1][C:2]1[NH:3][CH2:4][CH2:5][N:6]=1.C(N(CC)CC)C.Cl.[CH3:15][N:16]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23](Cl)=[O:24])[CH3:17]>ClCCl>[CH3:15][N:16]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]([N:6]1[CH2:5][CH2:4][N:3]=[C:2]1[CH3:1])=[O:24])[CH3:17]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 107982-MethylimidazolineHCID 21475509HCID 21475509, 화합물

생성물 1

HCID 70270103HCID 70270103, 화합물수율 66.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Dichloromethane (400 mL), 2-methyl-2-imidazoline (56.38 g, 0.637 mol), and triethylamine (283.51 g, 2.802 mol) are placed in a 2000 mL three-necked round bottomed flask equipped with a reflux condenser, internal thermometer, mechanical stirrer, addition funnel, and argon inlet. The solution is brought to reflux and 15 min later a solution of 6-(N,N-Dimethylamino)hexanoyl chloride.hydrochloride (150 g, 0.700 mol), prepared as described in example II, dissolved in dichloromethane (300 mL) is added dropwise over 45 min. The mixture is refluxed for an additional 2 h before being cooled to room temperature. The salts are filtered and washed with methylene chloride. The combined filtrates are washed with 5% NaHCO3 solution (3×300 mL) and water (300 mL). After drying over MgSO4 and filtration, the organic layer is concentrated first by rotary evaporation at 50° C. and then by Kugelrohr distillation at 60°-70° C. (0.2 mm Hg) to give 95.20 g (66%) of an oil which solidifies on standing.

후처리

  1. customequipped with a reflux condenser
  2. additioninternal thermometer, mechanical stirrer, addition funnel, and argon inlet
  3. customprepared
  4. additionis added dropwise over 45 min
  5. temperatureThe mixture is refluxed for an additional 2 h
  6. filtrationThe salts are filtered
  7. washwashed with methylene chloride
  8. washThe combined filtrates are washed with 5% NaHCO3 solution (3×300 mL) and water (300 mL)
  9. dry with materialAfter drying over MgSO4 and filtration
  10. concentrationthe organic layer is concentrated first by rotary evaporation at 50° C.
  11. distillationby Kugelrohr distillation at 60°-70° C. (0.2 mm Hg)

출처 및 근거

ORD 기록
ord-a160a818eb184201a3a2f07d2ee0ebf9
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05686015

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