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Triethylamine → 4-butoxy-N-(3-(5-phenylbenzo[d]isothiazol-3-ylamino)propyl) benzamide

HRID 502563
ノート
印刷プレビュー

反応式

HRID 502563 の反応式
[C:1]1([C:7]2[CH:8]=[CH:9][C:10]3[S:14][N:13]=[C:12]([NH:15][CH2:16][CH2:17][CH2:18][NH2:19])[C:11]=3[CH:20]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[CH2:28]([O:32][C:33]1[CH:41]=[CH:40][C:36]([C:37](Cl)=[O:38])=[CH:35][CH:34]=1)[CH2:29][CH2:30][CH3:31]>C(Cl)Cl>[CH2:28]([O:32][C:33]1[CH:34]=[CH:35][C:36]([C:37]([NH:19][CH2:18][CH2:17][CH2:16][NH:15][C:12]2[C:11]3[CH:20]=[C:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)[CH:8]=[CH:9][C:10]=3[S:14][N:13]=2)=[O:38])=[CH:40][CH:41]=1)[CH2:29][CH2:30][CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1185614-Butoxybenzoyl chlorideHCID 58727100N1-(5-Phenylbenzo[d]isothiazol-3-yl)propane-1,3-diamine

生成物 1

HCID 574364674-butoxy-N-(3-(5-phenylbenzo[d]isothiazol-3-ylamino)propyl) benzamide収率 14.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The crude N1-(5-Phenylbenzo[d]isothiazol-3-yl)propane-1,3-diamine mixture (˜100 mg, 0.20 mmol) was dissolved in anhydrous methylene chloride with triethylamine (0.3 mL, 0.24 mmol). The mixture was cooled in an ice-bath under nitrogen, then a solution of 4-butoxybenzoyl chloride (51 mg, 0.24 mmol) was added dropwise. After the addition was completed the ice-bath was removed and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with methylene chloride and then washed successively with saturated sodium bicarbonate solution and brine. The organic solution was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by prep-scale reverse phase high performance liquid chromatography to yield 4-butoxy-N-(3-(5-phenylbenzo[d]isothiazol-3-ylamino)propyl) benzamide (13 mg). 1H NMR (300 MHz, DMSO-d6): 8.23 (s, 1H), 8.17 (t, 1H), 7.98 (d, 1H), 7.76-7.82 (m, 4H), 7.50 (t, 3H), 7.37-7.40 (m, 1H), 6.97 (d, 2H), 4.00 (t, 2H), 3.50 (q, 2H), 3.39 (q, 2H), 1.90-2.00 (m, 2H), 1.62-1.78 (m, 2H), 1.40-1.49 (m, 2H), 0.96 ppm (t, 3H).

後処理

  1. temperatureThe mixture was cooled in an ice-bath under nitrogen
  2. additionAfter the addition
  3. customwas removed
  4. additionThe reaction mixture was diluted with methylene chloride
  5. washwashed successively with saturated sodium bicarbonate solution and brine
  6. dry with materialThe organic solution was dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe resulting residue was purified by prep-scale reverse phase high performance liquid chromatography

出典と根拠

ORDレコード
ord-97c1b835eaab4fc4adfeab85325aba3f
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776847B2

反応ノート

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