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Diisopropylethylamine → HCID 11597749, 화합물

HRID 2267424
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HRID 2267424 반응식
[CH2:1]([C:8]1[S:12][C:11]([C:13]2[C:18]([Cl:19])=[CH:17][N:16]=[C:15](SC)[N:14]=2)=[N:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.OOS([O-])=O.[K+].[NH2:28][CH2:29][CH2:30][N:31]1[C:35]([CH3:37])([CH3:36])[C:34](=[O:38])[NH:33][C:32]1=[O:39].C(N(C(C)C)CC)(C)C>CC(C)=O.O.CC(O)C>[CH2:1]([C:8]1[S:12][C:11]([C:13]2[C:18]([Cl:19])=[CH:17][N:16]=[C:15]([NH:28][CH2:29][CH2:30][N:31]3[C:35]([CH3:36])([CH3:37])[C:34](=[O:38])[NH:33][C:32]3=[O:39])[N:14]=2)=[N:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 81531DiisopropylethylamineHCID 23707502Potassium hydroxy sulfiteHCID 574288041-(2-Aminoethyl)-5,5-dimethylimidazolidine-2,4-dioneHCID 60204552HCID 60204552, 화합물

생성물 1

HCID 11597749HCID 11597749, 화합물수율 90.4%

시약·촉매·용매 3

HCID 180
Acetone
용매
2회
HCID 962Water용매
HCID 3776Isopropanol용매

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온도
170 °C

실험 절차

4-(5-Benzyl-1,3,4-thiadiazol-2-yl)-5-chloro-2-(methylthio)pyrimidine (0.190 g, 0.57 mmols) was dissolved in 75 mL acetone. Oxone (1.05 g, 1.7 mmol) was dissolved in 75 mL H2O and added to the acetone solution. This mixture was allowed to stir for 5 h. The acetone was removed under vacuum, the resulting precipitate was obtained by filtration. LC/MS analysis indicates a mixture of both sulfoxide and sulfone. This solid mixture was dried briefly in a vacuum oven. This material was charged to a microwave reaction vessel along with 1-(2-aminoethyl)-5,5-dimethyl-imidazolidine-2,4-dione (0.194 g, 1.1 mmol) and diisopropyl ethylamine (0.20 mL, 1.1 mmol) and 15 mL IPA. This reaction was heated under microwave conditions to 170° C. for 1200 s. Upon cooling 0.236 g (90% yield) of product was obtained by filtration. MS (M+H)+ 458.

후처리

  1. customThe acetone was removed under vacuum
  2. customthe resulting precipitate was obtained by filtration
  3. customThis solid mixture was dried briefly in a vacuum oven

출처 및 근거

ORD 기록
ord-d885369461f64d04a7707449eaa69443
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858785B2

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