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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
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HRID 1807634 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 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

생성물 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-carboxylate수율 86%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-9fb65f46fe1541bfa24dcfa01f38a11d
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08357687B2

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