Hydrochloric Acid → N-(4-azidophenylsulfonyl)-N'-(4-methoxy-6-methylpyrimidin-2-yl)urea

HRID 1583878ノート

反応式

HRID 1583878 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[N:6]=[C:5]([N:10](C2C=CC=CC=2)[C:11](=[O:13])[O-])[N:4]=1.[N:20]([C:23]1[CH:28]=[CH:27][C:26]([S:29]([NH2:32])(=[O:31])=[O:30])=[CH:25][CH:24]=1)=[N+:21]=[N-:22].N12CCCCC1C=NCCC2.Cl>O1CCOCC1.O>[N:20]([C:23]1[CH:28]=[CH:27][C:26]([S:29]([NH:32][C:11]([NH:10][C:5]2[N:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([CH3:9])[N:6]=2)=[O:13])(=[O:30])=[O:31])=[CH:25][CH:24]=1)=[N+:21]=[N-:22]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3141121,5-Diazabicyclo(5,4,0)undec-5-eneHCID 35585904-AzidobenzenesulfonamideHCID 18954641N-(4-methoxy-6-methylpyrimidin-2-yl)phenylcarbamate

生成物 1

HCID 23320462N-(4-azidophenylsulfonyl)-N'-(4-methoxy-6-methylpyrimidin-2-yl)urea収率 67%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of 2.9 g of N-(4-methoxy-6-methylpyrimidin-2-yl)phenylcarbamate in 10 ml of dioxan is added dropwise at 20°-25° C. to a solution of 2 g of 4-azidophenylsulfonamide and 1.6 ml of 1,5-diazabicyclo(5,4,0)-undec-5-ene in 20 ml of dioxan and the mixture is stirred for 3 hours at the same temperature. The reaction mixture is then taken up in 200 ml of water and the aqueous mixture is then acidified with hydrochloric acid to pH 2. The precipitated product is isolated, washed with ethyl acetate and dried, affording N-(4-azidophenylsulfonyl)-N'-(4-methoxy-6-methylpyrimidin-2-yl)urea in 67% yield in the form of greenish crystals with a melting point of 192° C.

後処理

  1. customThe precipitated product is isolated
  2. washwashed with ethyl acetate
  3. customdried

出典と根拠

ORDレコード
ord-2f73f91e51ff48b8ab8d1e842be3d9db
出典データセット
uspto-grants-1985_11
特許番号
US04555262

反応ノート

読み込み中…