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Bis(2-Methoxyethyl)amine → N,N-bis(2-methoxyethyl)sulfamoyl chloride

HRID 989690
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HRID 989690 반응식
[CH3:1][O:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][O:8][CH3:9].C(N(CC)CC)C.[S:17](Cl)([Cl:20])(=[O:19])=[O:18]>C(Cl)Cl>[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:6][CH2:7][O:8][CH3:9])[S:17]([Cl:20])(=[O:19])=[O:18]
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참가 물질

5

반응물 3

HCID 2383Bis(2-Methoxyethyl)amineHCID 8471TriethylamineHCID 24648Sulfuryl chloride

생성물 1

HCID 16228513N,N-bis(2-methoxyethyl)sulfamoyl chloride수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

A premixed solution of bis-methoxyethylamine (15.0 ml, 102 mmol, 1.00 equiv.) and triethylamine (21.3 ml, 153 mmol, 1.50 equiv.) was added dropwise to a solution of sulfuryl chloride (20.7 ml, 153 mmol, 1.50 equiv.) in CH2Cl2 at 0° C. The reaction mixture was continued stirred at 0° C. for 2 h, poured into ice and extracted with CH2Cl2 (3×100 ml). The combined organic extracts were washed with a saturated NaCl soln (1×100 ml), the organic layer dried (Na2SO4), filtered and concentrated under vacuum to afford the title compound (18.5 g, 80%) which was used without further purification. 1HNMR (CDCl3): 3.37 (s, 6H), 3.64-3.64 (m, 8H)

후처리

  1. additionpoured into ice
  2. extractionextracted with CH2Cl2 (3×100 ml)
  3. washThe combined organic extracts were washed with a saturated NaCl soln (1×100 ml)
  4. dry with materialthe organic layer dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-48d57fe7c7154dab91479dcf47e6ab78
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06458783B1

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