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Sulfamide → methyl 3-cyclohexyl-1-methyl-2-(2-{2-[methyl(2-{2-[methyl(sulfamoyl)amino]ethoxy}ethyl)amino]-2-oxoethoxy}phenyl)-1H-indole-6-carboxylate

HRID 1807634
ノート
印刷プレビュー

反応式

HRID 1807634 の反応式
[CH:1]1([C:7]2[C:15]3[C:10](=[CH:11][C:12]([C:16]([O:18][CH3:19])=[O:17])=[CH:13][CH:14]=3)[N:9]([CH3:20])[C:8]=2[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[O:27][CH2:28][C:29]([N:31]([CH3:39])[CH2:32][CH2:33][O:34][CH2:35][CH2:36][NH:37][CH3:38])=[O:30])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[S:40](N)([NH2:43])(=[O:42])=[O:41]>O1CCOCC1>[CH:1]1([C:7]2[C:15]3[C:10](=[CH:11][C:12]([C:16]([O:18][CH3:19])=[O:17])=[CH:13][CH:14]=3)[N:9]([CH3:20])[C:8]=2[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[O:27][CH2:28][C:29]([N:31]([CH3:39])[CH2:32][CH2:33][O:34][CH2:35][CH2:36][N:37]([CH3:38])[S:40](=[O:42])(=[O:41])[NH2:43])=[O:30])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 82267SulfamideHCID 67226641methyl 3-cyclohexyl-1-methyl-2-{2-[2-(methyl {2-[2-(methylamino)ethoxy]ethyl}amino)-2-oxoethoxy]phenyl}-1H-indole-6-carboxylate

生成物 1

HCID 58317822methyl 3-cyclohexyl-1-methyl-2-(2-{2-[methyl(2-{2-[methyl(sulfamoyl)amino]ethoxy}ethyl)amino]-2-oxoethoxy}phenyl)-1H-indole-6-carboxylate収率 86%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of intermediate 6 (620 mg, 1.16 mmol) and sulfamide (900 mg, 9.36 mmol) in dioxane (10 mL) was heated at 100° C. in a microwave oven for 60 minutes. The reaction mixture was cooled down to room temperature, and then evaporated under vacuum. The residue was triturated in water, filtered and washed with water. The powder was reconstituted in AcOEt. The solution was dried over anhydrous Na2SO4, filtered and the filtrate evaporated to yield 610 mg (86%) of methyl 3-cyclohexyl-1-methyl-2-(2-{2-[methyl(2-{2-[methyl(sulfamoyl)amino]ethoxy}ethyl)amino]-2-oxoethoxy}phenyl)-1H-indole-6-carboxylate 7 as a yellowish powder: m/z=615 (M+H)+.

後処理

  1. customevaporated under vacuum
  2. customThe residue was triturated in water
  3. filtrationfiltered
  4. washwashed with water
  5. dry with materialThe solution was dried over anhydrous Na2SO4
  6. filtrationfiltered
  7. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-9fb65f46fe1541bfa24dcfa01f38a11d
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08357687B2

反応ノート

読み込み中…

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