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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Diethyl Ether → N'-(2-Amino-2-methylpropyl)-N,N-dimethylsulfuric diamide

HRID 1381939
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인쇄 미리보기

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HRID 1381939 반응식
[NH2:1][CH2:2][C:3]([NH2:6])([CH3:5])[CH3:4].CCOCC.[CH3:12][N:13]([CH3:18])[S:14](Cl)(=[O:16])=[O:15]>C(N(CC)CC)C>[CH3:4][C:3]([NH2:6])([CH3:5])[CH2:2][NH:1][S:14]([N:13]([CH3:18])[CH3:12])(=[O:16])=[O:15]
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참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 131282-MethylpropylenediamineHCID 83372Dimethylsulphamoyl chloride

생성물 1

HCID 13603865N'-(2-Amino-2-methylpropyl)-N,N-dimethylsulfuric diamide수율 60.4%

시약·촉매·용매 1

HCID 8471Triethylamine용매

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온도
0 °C

실험 절차

A mixture of 30.7 g (0.35 mole) of 1,2-diamino-2-methylpropane, 150 ml of ether and 50 ml of triethylamine was cooled to 0° C. and 20 g (0.14 mole) of dimethylsulfamoylchloride was added slowly. The mixture was stirred for 30 min. and then concentrated under reduced pressure. The residue was mised with water, basified with potassium carbonate and concentrated to dryness. Acetone was added and insoluble material was removed by filtration. Concentration of the filtrate gave a solid, which crystallized from toluene to give 16.5 g (60%) of product, m.p. 77°-78° C. The IR and MNR spectra were consistent with the assigned structure.

후처리

  1. concentrationconcentrated under reduced pressure
  2. concentrationconcentrated to dryness
  3. additionAcetone was added
  4. custominsoluble material was removed by filtration
  5. customConcentration of the filtrate gave a solid, which
  6. customcrystallized from toluene

출처 및 근거

ORD 기록
ord-4a7e1ef0a87f477085251163eaa5856a
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04804677

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