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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
ノート
印刷プレビュー

反応式

HRID 728793 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cbcb97c9fb964c509df9014094a62037
出典データセット
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05051420

反応ノート

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