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Sodium Hydroxide → S-[2-(diethylamino)ethyl]-S-[4-(1H-imidazol-1-yl)-1,2,5-thiadiazol-3-yl]sulfoximine

HRID 728793
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HRID 728793 반응식
CCC(CCCCC([NH:11]C(C(NC(C(NC(C(NC1C(=O)NC(CCN)C(=O)NC(CC2C=CC=CC=2)C(=O)NC(CC(C)C)C(=O)NC(CCN)C(=O)NC(CCN)C(=O)NC(C(O)C)C(=O)NCC1)=O)CCN)=O)C(O)C)=O)CCN)=O)C.OS(O)(=O)=O.[CH2:91]([N:93]([CH2:108][CH3:109])[CH2:94][CH2:95][S:96]([C:98]1[C:102]([N:103]2[CH:107]=[CH:106][N:105]=[CH:104]2)=[N:101][S:100][N:99]=1)=[O:97])[CH3:92].[N-]=[N+]=[N-].[Na+].[OH-].[Na+]>C(Cl)(Cl)Cl.O>[CH2:108]([N:93]([CH2:91][CH3:92])[CH2:94][CH2:95][S:96]([C:98]1[C:102]([N:103]2[CH:107]=[CH:106][N:105]=[CH:104]2)=[N:101][S:100][N:99]=1)(=[NH:11])=[O:97])[CH3:109]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 33557Sodium AzideHCID 5702105AerosporinHCID 67945728N,N-diethyl-2-[[4-(1H-imidazol-1-yl)-1,2,5-thiadiazol-3-yl]sulfinyl]-ethanamine

생성물 1

HCID 57202344S-[2-(diethylamino)ethyl]-S-[4-(1H-imidazol-1-yl)-1,2,5-thiadiazol-3-yl]sulfoximine

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6212Chloroform용매

실험 절차

Concentrated sufuric acid (13 ml) is added dropwise to a stirred slurry of the compound of Example 11 (13 mmol) and sodium azide (52 mmol) in chloroform at -20° C. The reaction mixture is allowed to warm to ambient temperature and then heated at reflux temperature for 36 hr. The reaction mixture is then cooled to 0° C. and water (100 ml) added. The mixture is carefully basified with 50% sodium hydroxide solution. The chloroform layer is separated and the aqueous layer is extracted with methylene chloride. The combined organic layers are dried and concentratedto obtain the product which is purified by standard procedures.

후처리

  1. temperatureheated
  2. temperatureat reflux temperature for 36 hr
  3. temperatureThe reaction mixture is then cooled to 0° C.
  4. customThe chloroform layer is separated
  5. extractionthe aqueous layer is extracted with methylene chloride
  6. customThe combined organic layers are dried
  7. customconcentratedto obtain the product which
  8. customis purified by standard procedures

출처 및 근거

ORD 기록
ord-cbcb97c9fb964c509df9014094a62037
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05051420

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