Hydrochloric Acid → HCID 14346756、化合物

HRID 622598ノート

反応式

HRID 622598 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[S:10]([NH2:13])(=[O:12])=[O:11])[CH:3]=[CH:2]1.C[O:15][C:16](=O)[NH:17][C:18]1[N:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([CH3:26])[N:19]=1.C[Al](C)C.Cl>C(Cl)Cl.C1(C)C=CC=CC=1>[CH3:25][O:24][C:22]1[CH:21]=[C:20]([CH3:26])[N:19]=[C:18]([NH:17][C:16]([NH:13][S:10]([C:8]2[CH:7]=[CH:6][CH:5]=[C:4]3[C:9]=2[NH:1][CH:2]=[CH:3]3)(=[O:11])=[O:12])=[O:15])[N:23]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 13072161Methyl (4-methoxy-6-methylpyrimidin-2-yl)carbamateHCID 143467551H-Indole-7-sulfonamideHCID 16682925Trimethylaluminum

生成物 1

HCID 14346756HCID 14346756、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1H-indole-7-sulfonamide (1.0 g) and (4-methoxy-6-methylpyrimidin-2-yl)carbamic acid methyl ester (1.0 g) in methylene chloride (100 ml) was added trimethylaluminum (3.2 ml of a 2.0M solution in toluene). The mixture was heated at reflux for 18 hours under a nitrogen atmosphere. Work-up was achieved by careful addition of 100 ml of 1N HCl followed by separation of the organic layer. The methylene chloride was dried over MgSO4 and evaporated to an oil. The oil was dissolved in ether from which it quickly crystallized to give pure product (TLC) (0.56 g, m.p. 207°-209° C.).

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 18 hours under a nitrogen atmosphere
  3. customfollowed by separation of the organic layer
  4. dry with materialThe methylene chloride was dried over MgSO4
  5. customevaporated to an oil
  6. dissolutionThe oil was dissolved in ether from which it
  7. customquickly crystallized
  8. customto give pure product (TLC) (0.56 g, m.p. 207°-209° C.)

出典と根拠

ORDレコード
ord-b61df04323384fe7ba233196ac2ec72e
出典データセット
uspto-grants-1988_09
特許番号
US04772313

反応ノート

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