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Sulfuric Acid → N,N-diethyl-2-[[4-(1H-imidazol-1-yl)-1,2,5-thiadiazol-3-yl]sulfinyl]-ethanamine

HRID 728792
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HRID 728792 반응식
[CH2:1]([N:3]([CH2:17][CH3:18])[CH2:4][CH2:5][S:6][C:7]1[C:11]([N:12]2[CH:16]=[CH:15][N:14]=[CH:13]2)=[N:10][S:9][N:8]=1)[CH3:2].S(=O)(=O)(O)[OH:20].B1([O-])OO1.O.O.O.O.[Na+]>CO>[CH2:17]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][S:6]([C:7]1[C:11]([N:12]2[CH:16]=[CH:15][N:14]=[CH:13]2)=[N:10][S:9][N:8]=1)=[O:20])[CH3:18]
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참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 23693097Sodium;3-oxidodioxaborirane;tetrahydrateHCID 67945755HCID 67945755, 화합물

생성물 1

HCID 67945728N,N-diethyl-2-[[4-(1H-imidazol-1-yl)-1,2,5-thiadiazol-3-yl]sulfinyl]-ethanamine

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

A cold (0° C.) solution of the compound of Example 10 in methanol istreated slowly with excess 30% sulfuric acid an then sodium perborate tetrahydrate (10 equivalents) is added. The mixture is stirred at 0° C. for 2 hrs and then at ambient temperature for 2 hrs. The methanol is removed in vacuo and the residue basified with 50% sodium hydroxide and filtered. The filter cake is washed with methylene chloride and the aqueous filtrate extracted with the methylene chloride washings. The combined extract is washed with water, dried, and concentrated to obtain the title compound.

후처리

  1. additionis added
  2. waitat ambient temperature for 2 hrs
  3. customThe methanol is removed in vacuo
  4. filtrationfiltered
  5. washThe filter cake is washed with methylene chloride
  6. extractionthe aqueous filtrate extracted with the methylene chloride washings
  7. extractionThe combined extract
  8. washis washed with water
  9. customdried
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4b1cdf44a63645debeac2295d681d741
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05051420

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