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Ethyl Propionate → 5-bromo-1-(toluene-4-sulfonyl)-6-trifluoromethyl-1H-indole-2-carboxylic acid ethyl ester

HRID 74465
ノート
印刷プレビュー

反応式

HRID 74465 の反応式
C(N(CC)C(C)C)(C)C.[C:10]([O:14][CH2:15][CH3:16])(=[O:13])[CH2:11][CH3:12].[Br:17][C:18]1[C:23]([C:24]([F:27])([F:26])[F:25])=[CH:22][C:21]([NH:28][S:29]([C:32]2[CH:37]=[CH:36][C:35]([CH3:38])=[CH:34][CH:33]=2)(=[O:31])=[O:30])=[C:20](I)[CH:19]=1>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[Br-].[Zn+2].[Br-].O1CCCC1>[CH2:15]([O:14][C:10]([C:11]1[N:28]([S:29]([C:32]2[CH:33]=[CH:34][C:35]([CH3:38])=[CH:36][CH:37]=2)(=[O:31])=[O:30])[C:21]2[C:20]([CH:12]=1)=[CH:19][C:18]([Br:17])=[C:23]([C:24]([F:27])([F:25])[F:26])[CH:22]=2)=[O:13])[CH3:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 7749Ethyl PropionateHCID 81531DiisopropylethylamineHCID 68005027N-(4-bromo-2-iodo-5-trifluoromethyl-phenyl)-4-methyl-benzenesulfonamide

生成物 1

HCID 680047005-bromo-1-(toluene-4-sulfonyl)-6-trifluoromethyl-1H-indole-2-carboxylic acid ethyl ester

試薬・触媒・溶媒 3

HCID 10421208Zinc bromide触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

N,N-diisopropylethyl amine (0.42 ml, 2.4 mmol), ethyl propionate (0.12 ml, 1.2 mmol), and tetrakis(triphenylphosphine)palladium (46 mg, 0.04 mmol) were added to an anhydrous tetrahydrofuran (THF) solution (3.2 ml) containing N-(4-bromo-2-iodo-5-trifluoromethyl-phenyl)-4-methyl-benzenesulfonamide (208 mg, 0.4 mmol) and zinc bromide (270 mg, 1.2 mmol). Then, the mixture was evacuated, and backfilled with argon. This was stirred at 80° C. for 13 hours. After cooling it to room temperature, the reaction mixture was filtered through Celite, and washed with ethyl acetate. The wash solution was washed with an aqueous solution saturated with sodium bicarbonate and an aqueous solution saturated with sodium chloride, and dried over anhydrous sodium sulfate. The desiccant was removed by filtration, and concentration was performed. Then, the residue obtained by concentration under reduced pressure was purified by silica gel column chromatography. Thus, 5-bromo-1-(toluene-4-sulfonyl)-6-trifluoromethyl-1H-indole-2-carboxylic acid ethyl ester was obtained as a pale brown solid (195 mg, 50%).

後処理

  1. customThen, the mixture was evacuated
  2. temperatureAfter cooling it to room temperature
  3. filtrationthe reaction mixture was filtered through Celite
  4. washwashed with ethyl acetate
  5. washThe wash solution was washed with an aqueous solution saturated with sodium bicarbonate
  6. dry with materialan aqueous solution saturated with sodium chloride, and dried over anhydrous sodium sulfate
  7. customThe desiccant was removed by filtration, and concentration
  8. customThen, the residue obtained by concentration under reduced pressure
  9. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-bd000ac9664b45088171998e60399da1
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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