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Diisopropylethylamine → HCID 11597749、化合物

HRID 2267424
ノート
印刷プレビュー

反応式

HRID 2267424 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

HCID 11597749HCID 11597749、化合物収率 90.4%

試薬・触媒・溶媒 3

HCID 180
Acetone
溶媒
2 回
HCID 962Water溶媒
HCID 3776Isopropanol溶媒

反応条件

温度
170 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d885369461f64d04a7707449eaa69443
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858785B2

反応ノート

読み込み中…

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