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Pyrrolidine → 2-Dimethylamino-6-methoxybenzo[b]thiophen-3-yl 4-[(1-Pyrrolidinyl)methyl]phenyl Ketone

HRID 1387018
ノート
印刷プレビュー

反応式

HRID 1387018 の反応式
Cl[CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1.[CH3:12][N:13]([CH3:25])[C:14]1[S:18][C:17]2[CH:19]=[C:20]([O:23][CH3:24])[CH:21]=[CH:22][C:16]=2[CH:15]=1.[NH:26]1[CH2:30][CH2:29][CH2:28][CH2:27]1>ClC1C=CC=CC=1>[N:26]1([CH2:2][C:3]2[CH:11]=[CH:10][C:6]([C:7]([C:15]3[C:16]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:17]=4[S:18][C:14]=3[N:13]([CH3:25])[CH3:12])=[O:8])=[CH:5][CH:4]=2)[CH2:30][CH2:29][CH2:28][CH2:27]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

5

反応物 3

HCID 31268PyrrolidineHCID 701364-(Chloromethyl)benzoyl chlorideHCID 105125306-Methoxy-N,N-dimethylbenzo[b]thiophen-2-amine

生成物 1

HCID 211827022-Dimethylamino-6-methoxybenzo[b]thiophen-3-yl 4-[(1-Pyrrolidinyl)methyl]phenyl Ketone収率 74%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

反応条件

温度
0 °C

実験手順

4-(Chloromethyl)benzoyl chloride (105 mg, 0.558 mmol) was added to a stirred solution of 2-dimethylamino-6-methoxybenzo[b]thiophene (105 mg, 0.507 mmol) in chlorobenzene (1 mL) under nitrogen. The resultant mixture was heated in an oil bath at 110° C. for 2.5 h. The mixture was cooled to 0° C., treated with pyrrolidine (5 mL), then allowed to stir at room temperature for 2 h. After dilution with THF (20 mL), the mixture was washed with saturated aqueous NaHCO3 (5 mL). The organic layer was dried over MgSO4, filtered, concentrated, and chromatographed on silica [gradient 20-40% EtOAc in hexanes, then 0-10% EtOH/Et3N (2/1) in THF/hexanes (1/1)] to give 148 mg (74%) of the ketone as a foam.

後処理

  1. washAfter dilution with THF (20 mL), the mixture was washed with saturated aqueous NaHCO3 (5 mL)
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customchromatographed on silica [gradient 20-40% EtOAc in hexanes

出典と根拠

ORDレコード
ord-01d69db52bdf454d9401912001aada42
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06265575B1

反応ノート

読み込み中…

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