Hydrochloric Acid → HCID 20195202、化合物

HRID 653207ノート

反応式

HRID 653207 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([S:14](=[O:17])(=[O:16])[NH2:15])[C:5]2[O:10][S:9](=[O:12])(=[O:11])[CH:8]=[CH:7][C:6]=2[CH:13]=1.[CH3:18][O:19][C:20]1[CH:25]=[C:24]([O:26][CH3:27])[N:23]=[C:22]([N:28](C2C=CC=CC=2)[C:29](=O)[O-:30])[N:21]=1.N12CCCN=C1CCCCC2.Cl>C(#N)C.O>[Br:1][C:2]1[CH:3]=[C:4]([S:14]([NH:15][C:29]([NH:28][C:22]2[N:21]=[C:20]([O:19][CH3:18])[CH:25]=[C:24]([O:26][CH3:27])[N:23]=2)=[O:30])(=[O:17])=[O:16])[C:5]2[O:10][S:9](=[O:12])(=[O:11])[CH:8]=[CH:7][C:6]=2[CH:13]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 20195198HCID 20195198、化合物HCID 22104197HCID 22104197、化合物

生成物 1

HCID 20195202HCID 20195202、化合物収率 65.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

0.3 g of 6-bromo-8-sulfamoyl-2,2-dioxo-1,2-benzoxathiine are dissolved in 10 ml of acetonitrile. To this solution are added 0.25 g of N-(4,6-dimethoxypyrimidin-2-yl)phenylcarbamate and 0.15 g of 1,8-diazabicyclo[5.4.0]undec-7-ene and the mixture is stirred for 2 hours at 20°-25° C. The mixture is then acidified with 5% hydrochloric acid and diluted with water. The precipitated oil is extracted with ethyl acetate and the combined organic phases are washed with water, dried and concentrated. The oily residue is crystallised from ether, affording 0.3 g of N-(6-bromo-2,2-dioxo-1,2-benzoxathiin-8-ylsulfonyl)-N'-(4,6-dimethoxypyrimidin-2-yl)urea of m.p. 204°-209° C. (decompos.).

後処理

  1. extractionThe precipitated oil is extracted with ethyl acetate
  2. washthe combined organic phases are washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe oily residue is crystallised from ether

出典と根拠

ORDレコード
ord-69aad464434442179393841216b535ef
出典データセット
uspto-grants-1987_06
特許番号
US04675417

反応ノート

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