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Hydrochloric Acid → 2,3-Dihydro-N-[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]-2-methyl-1H-indole-7-sulfonamide

HRID 622596
ノート
印刷プレビュー

反応式

HRID 622596 の反応式
[CH3:1][CH:2]1[CH2:10][C:9]2[C:4](=[C:5]([S:11]([NH2:14])(=[O:13])=[O:12])[CH:6]=[CH:7][CH:8]=2)[NH:3]1.C[O:16][C:17](=O)[NH:18][C:19]1[N:24]=[C:23]([O:25][CH3:26])[CH:22]=[C:21]([CH3:27])[N:20]=1.C[Al](C)C.Cl>C(Cl)Cl.C1(C)C=CC=CC=1>[CH3:26][O:25][C:23]1[CH:22]=[C:21]([CH3:27])[N:20]=[C:19]([NH:18][C:17]([NH:14][S:11]([C:5]2[CH:6]=[CH:7][CH:8]=[C:9]3[C:4]=2[NH:3][CH:2]([CH3:1])[CH2:10]3)(=[O:13])=[O:12])=[O:16])[N:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 13072161Methyl (4-methoxy-6-methylpyrimidin-2-yl)carbamateHCID 143467302,3-dihydro-2-methyl-1H-indole-7-sulfonamideHCID 16682925Trimethylaluminum

生成物 1

HCID 143467312,3-Dihydro-N-[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]-2-methyl-1H-indole-7-sulfonamide収率 11.2%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2,3-dihydro-2-methyl-1H-indole-7-sulfonamide (1.0 g) and (4-methoxy-6-methylpyrimidin-2-yl)carbamic acid methyl ester (1.0 g) in methylene dichloride (100 ml) was added trimethylaluminum (3.0 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 dryness. The residue was chromatographed on a silica gel column to give the pure product (0.2 g, m.p. 175°-177° 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 dryness
  6. customThe residue was chromatographed on a silica gel column

出典と根拠

ORDレコード
ord-5581de56a805477eafe495c58db8a727
出典データセット
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04772313

反応ノート

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