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1,1'-Carbonyldiimidazole → 7-chloro-3-{1-[2-(2-methyl-5-nitrophenyl)-1-oxoethyl]-piperidin-4-yl}-1H-indole

HRID 351771
ノート
印刷プレビュー

反応式

HRID 351771 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH2:11][C:12]([OH:14])=O.C(N1C=CN=C1)(N1C=CN=C1)=O.[Cl:27][C:28]1[CH:29]=[CH:30][CH:31]=[C:32]2[C:36]=1[NH:35][CH:34]=[C:33]2[CH:37]1[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]1>CN(C)C=O.O1CCCC1>[Cl:27][C:28]1[CH:29]=[CH:30][CH:31]=[C:32]2[C:36]=1[NH:35][CH:34]=[C:33]2[CH:37]1[CH2:42][CH2:41][N:40]([C:12](=[O:14])[CH2:11][C:3]2[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=2[CH3:1])[CH2:39][CH2:38]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 120720367-chloro-3-(piperidin-4-yl)-1H-indoleHCID 224753382-(2-Methyl-5-nitrophenyl)acetic acid

生成物 1

HCID 227144217-chloro-3-{1-[2-(2-methyl-5-nitrophenyl)-1-oxoethyl]-piperidin-4-yl}-1H-indole収率 89.3%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回
HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of (2-methyl-5-nitrophenyl)acetic acid (2.5 g) and 1,1′-carbonyldiimidazole (2.1 g) in dimethyl formamide (50 mL) was stirred at room temperature for 15 min and subsequently added a solution of 7-chloro-3-(piperidin-4-yl)-1H-indole (3.0 g) in dimethyl formamide (50 mL). The resulting mixture was stirred at room temperature for 1 h and poured onto an ice/water mixture. The compound was isolated by filtration and dissolved in tetrahydrofuran. The organic phase was washed with brine, dried (MgSO4), filtered and concentrated in vacuo to give 7-chloro-3-{1-[2-(2-methyl-5-nitrophenyl)-1-oxoethyl]-piperidin-4-yl}-1H-indole (4.7 g). A mixture of 7-chloro-3-{1-[2-(2-methyl-5-nitrophenyl)-1-oxoethyl]-piperidin-4-yl}-1H-indole (16.6 g) and ethanol (500 mL) was heated to reflux temperature and subsequently added concentrated HCl (22 mL) and iron powder (11.3 g) over a period of 30 min. The resulting mixture was boiled under reflux for an additional 90 min, filtered hot and concentrated in vacuo. The residue was dissolved in tetrahydrofuran, and the organic phase was washed with brine, dried (MgSO4), filtered and concentrated in vacuo to give give 7-chloro-3-{1-[2-(5-amino-2-methylphenyl)-1-oxoethyl]-piperidin-4-yl}-1H-indole (14.3 g). A suspension of lithium aluminium hydride (6.4 g) in tetrahydrofuran (250 mL) was cooled (5° C.) and subsequently added a mixture of 7-chloro-3-{1-[2-(5-amino-2-methylphenyl)-1-oxoethyl]-piperidin-4-yl}-1H-indole (16.0 g) in tetrahydrofuran (250 mL). The resulting mixture was boiled under reflux for 90 min, cooled to 5° C. and quenched by the addition of water. The mixture was dried (MgSO4), stirred for 10 min, filtered and concentrated in vacuo to give 7-chloro-3-{1-[2-(5-amino-2-methylphenyl)ethyl]piperidin-4-yl}-1H-indole (12.4 g). A solution of 7-chloro-3-{1-[2-(5-amino-2-methylphenyl)ethyl]piperidin-4-yl}-1H-indole (1.0 g) and N-ethyldiisopropylamine (0.7 g) in tetrahydrofuran (25 mL) was cooled (5° C.) and subsequently added a solution of (4-fluorophenyl)acetyl chloride in tetrahydrofuran (25 mL). The resulting mixture was stirred at room temperature for 1 h and subsequently poured onto brine. The aqueous phase was extracted with tetrahydrofuran, and the combined organic phases were dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by flash chromatography on silicagel (eluent:ethyl acetate/heptane/triethylamine 70:30:5) to give the product (0.81 g). LC/MS (m/z) 504 (MH+), RT=2.45, purity: 62%.

後処理

  1. stirringThe resulting mixture was stirred at room temperature for 1 h
  2. customThe compound was isolated by filtration
  3. washThe organic phase was washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-ab075b5fa896412d86ab8c47b4d7ea78
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06743809B2

反応ノート

読み込み中…

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