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Tryptamine → 2-[4-dimethylamino-4-(4-fluorophenyl)cyclohexylidene]-N-[2-(1H-indol-3-yl)ethyl]acetamide

HRID 908947
ノート
印刷プレビュー

反応式

HRID 908947 の反応式
ON1C2C=CC=CC=2N=N1.[NH2:11][CH2:12][CH2:13][C:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[NH:16][CH:15]=1.CN1CCOCC1.Cl.[CH3:31][N:32]([CH3:50])[C:33]1([C:43]2[CH:48]=[CH:47][C:46]([F:49])=[CH:45][CH:44]=2)[CH2:38][CH2:37][C:36](=[CH:39][C:40](O)=[O:41])[CH2:35][CH2:34]1.C1(N=C=NC2CCCCC2)CCCCC1.[OH-].[Na+]>O.CN(C)C=O>[CH3:50][N:32]([CH3:31])[C:33]1([C:43]2[CH:44]=[CH:45][C:46]([F:49])=[CH:47][CH:48]=2)[CH2:38][CH2:37][C:36](=[CH:39][C:40]([NH:11][CH2:12][CH2:13][C:14]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[NH:16][CH:15]=2)=[O:41])[CH2:35][CH2:34]1
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

9

反応物 6

HCID 1150TryptamineHCID 79724-MethylmorpholineHCID 10868DicyclohexylcarbodiimideHCID 14798Sodium HydroxideHCID 757711-HydroxybenzotriazoleHCID 67386287HCID 67386287、化合物

生成物 1

HCID 11705178
2-[4-dimethylamino-4-(4-fluorophenyl)cyclohexylidene]-N-[2-(1H-indol-3-yl)ethyl]acetamide
収率 95%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

1-Hydroxybenzotriazole (864 mg, 6.4 mmol), tryptamine (512 mg, 3.2 mmol) and N-methylmorpholine (0.703 ml, 6.4 mmol) were added to a solution of (4-dimethylamino-4-(4-fluorophenyl)cyclohexylidene)acetic acid hydrochloride (840 mg, 3.2 mmol) in abs. dimethylformamide (25 ml) under argon. The solution was cooled to 0° C., dicyclohexylcarbodiimide (1.32 g, 6.4 mmol) was added and the mixture was stirred at RT for 4 d. Working up of the mixture was carried out by separating off the urea which had precipitated out and introducing the filtrate into a mixture of saturated NaCl solution (40 ml) and saturated NaHCO3 solution (10 ml). Still further urea thereby precipitated out and was separated off. The filtrate was diluted with water (400 ml), 5 M sodium hydroxide solution (5 ml, 25 mmol) was added and the mixture was stored at 5° C. for 4 d. The product thereby precipitated out as a beige-coloured oily solid in a yield of 95% (1.27 mg).

後処理

  1. customby separating off the urea which
  2. customhad precipitated out
  3. additionintroducing the filtrate
  4. additioninto a mixture of saturated NaCl solution (40 ml) and saturated NaHCO3 solution (10 ml)
  5. customStill further urea thereby precipitated out and
  6. customwas separated off
  7. additionwas added
  8. waitthe mixture was stored at 5° C. for 4 d
  9. customThe product thereby precipitated out as a beige-coloured oily solid in a yield of 95% (1.27 mg)

出典と根拠

ORDレコード
ord-dbf86c35b6574955bf25d73aa75aa925
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08017630B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート