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Acetic Acid → 5-(1-isopropyl-piperidin-4-yl)-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester

HRID 74476
ノート
印刷プレビュー

反応式

HRID 74476 の反応式
Cl.[CH2:2]([O:4][C:5]([C:7]1[N:8]([S:22]([C:25]2[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=2)(=[O:24])=[O:23])[C:9]2[C:14]([CH:15]=1)=[CH:13][C:12]([CH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)=[CH:11][CH:10]=2)=[O:6])[CH3:3].C(N(CC)CC)C.[CH3:39][C:40]([CH3:42])=O.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)(O)[O-].[Na+]>ClC(Cl)C>[CH2:2]([O:4][C:5]([C:7]1[N:8]([S:22]([C:25]2[CH:26]=[CH:27][C:28]([CH3:31])=[CH:29][CH:30]=2)(=[O:23])=[O:24])[C:9]2[C:14]([CH:15]=1)=[CH:13][C:12]([CH:16]1[CH2:21][CH2:20][N:19]([CH:40]([CH3:42])[CH3:39])[CH2:18][CH2:17]1)=[CH:11][CH:10]=2)=[O:6])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 176Acetic AcidHCID 180AcetoneHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 680052465-piperidin-4-yl-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester hydrochloride

生成物 1

HCID 68005217
5-(1-isopropyl-piperidin-4-yl)-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

A mixture of 5-piperidin-4-yl-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester hydrochloride (253 mg, 0.592 mmol) in dichloroethane (4 ml), triethylamine (0.17 ml, 1.18 mmol), acetone (1.44 ml, 19.6 mmol), acetic acid (0.28 ml, 4.89 mmol), and sodium triacetoxyborohydride (318 mg, 1.50 mmol) was stirred at room temperature for 14.5 hours. The pH of the reaction mixture was adjusted to 9 (basic) using an aqueous solution saturated with sodium bicarbonate. The mixture was extracted with ethyl acetate. The extract was washed with an aqueous solution saturated with sodium chloride, and then dried over anhydrous sodium sulfate. The desiccant was removed by filtration, and concentration was performed. The resulting residue was purified by amino gel column chromatography (hexane/ethyl acetate=92/8 to 35/65). Thus, 5-(1-isopropyl-piperidin-4-yl)-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester was obtained as a colorless gum-like material (191 mg, 69%).

後処理

  1. extractionThe mixture was extracted with ethyl acetate
  2. washThe extract was washed with an aqueous solution saturated with sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe desiccant was removed by filtration, and concentration
  5. customThe resulting residue was purified by amino gel column chromatography (hexane/ethyl acetate=92/8 to 35/65)

出典と根拠

ORDレコード
ord-1d42c6a62ba648a69c404144ffb5b899
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829199B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート