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Potassium Iodide → (6-((Methylsulfonyl)oxy)-2-(4-((methylsulfonyl)oxy)phenyl)benzo(b)thien-3-yl)(4-(2-(1-piperidinyl)ethoxy)phenyl)-, hydrochloride

HRID 1649607
ノート
印刷プレビュー

反応式

HRID 1649607 の反応式
[CH3:1][S:2]([O:5][C:6]1[CH:7]=[CH:8][C:9]2[C:13]([C:14](=[O:25])[C:15]3[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][Cl:24])=[CH:17][CH:16]=3)=[C:12]([C:26]3[CH:31]=[CH:30][C:29]([O:32][S:33]([CH3:36])(=[O:35])=[O:34])=[CH:28][CH:27]=3)[S:11][C:10]=2[CH:37]=1)(=[O:4])=[O:3].[NH:38]1[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]1.[I-].[K+]>CN(C)C=O>[ClH:24].[CH3:1][S:2]([O:5][C:6]1[CH:7]=[CH:8][C:9]2[C:13]([C:14](=[O:25])[C:15]3[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][N:38]4[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]4)=[CH:17][CH:16]=3)=[C:12]([C:26]3[CH:31]=[CH:30][C:29]([O:32][S:33]([CH3:36])(=[O:35])=[O:34])=[CH:28][CH:27]=3)[S:11][C:10]=2[CH:37]=1)(=[O:4])=[O:3]
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 4875Potassium IodideHCID 8082PiperidineHCID 204789706-Methanesulfonyloxy-2-(4-methanesulfonyloxyphenyl)-3-[4-(2-chloroethoxy)benzoyl]benzo[b]thiophene

生成物 1

HCID 19603580(6-((Methylsulfonyl)oxy)-2-(4-((methylsulfonyl)oxy)phenyl)benzo(b)thien-3-yl)(4-(2-(1-piperidinyl)ethoxy)phenyl)-, hydrochloride

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

An 0.58 g. portion of 6-methanesulfonyloxy-2-(4-methanesulfonyloxyphenyl)-3-[4-(2-chloroethoxy)-benzoyl]benzo[b]thiophene was combined with 20 ml. of dimethylformamide, 4.8 ml. of piperidine and 100 mg. of potassium iodide, and the mixture was stirred overnight at 40° C. and then at 50° C. for two hours. The mixture was evaporated to a brown oil under vacuum, and the oil was worked up by pouring it into 50 ml. of saturated aqueous sodium bicarbonate and extracting the mixture twice with 40 ml. portions of ethyl acetate. The organic layers were combined, washed twice with 100 ml. portions of saturated aqueous sodium chloride and concentrated under vacuum to an oil. To the oily residue was added 50 ml. of 3% hydrogen chloride in methanol, and the acidic mixture was concentrated again to an oil, which was dissolved in hot denatured ethanol and crystallized. The first crop of purified crystals amounted to 0.4 g. and had a melting point and infrared and ultraviolet spectra identical to those of the products of Preparations 8 and 11.

後処理

  1. customThe mixture was evaporated to a brown oil under vacuum
  2. additionby pouring it into 50 ml
  3. extractionof saturated aqueous sodium bicarbonate and extracting the mixture twice with 40 ml
  4. washwashed twice with 100 ml
  5. concentrationportions of saturated aqueous sodium chloride and concentrated under vacuum to an oil
  6. additionTo the oily residue was added 50 ml
  7. concentrationof 3% hydrogen chloride in methanol, and the acidic mixture was concentrated again to an oil, which
  8. dissolutionwas dissolved in hot denatured ethanol
  9. customcrystallized

出典と根拠

ORDレコード
ord-d05128123e19410a8296b99edaccf687
出典データセット
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04418068

反応ノート

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