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Hydrochloric Acid → (R)-1-(3-(9H-Tribenz[b,d,f]azepine-9-yl)propyl)-3-piperidinecarboxylic acid, hydrochloride

HRID 861899
ノート
印刷プレビュー

反応式

HRID 861899 の反応式
[ClH:1].C([O:4][C:5]([C@@H:7]1[CH2:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][CH2:15][N:16]2[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[C:20]3[CH:27]=[CH:28][CH:29]=[CH:30][C:19]=3[C:18]3[CH:31]=[CH:32][CH:33]=[CH:34][C:17]2=3)[CH2:8]1)=[O:6])C.Cl>C(O)C.[OH-].[Na+]>[ClH:1].[CH:30]1[C:19]2[C:18]3[CH:31]=[CH:32][CH:33]=[CH:34][C:17]=3[N:16]([CH2:15][CH2:14][CH2:13][N:9]3[CH2:10][CH2:11][CH2:12][C@@H:7]([C:5]([OH:6])=[O:4])[CH2:8]3)[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[C:20]=2[CH:27]=[CH:28][CH:29]=1
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 2

HCID 313Hydrochloric AcidHCID 70197521(R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride

生成物 1

HCID 131720461(R)-1-(3-(9H-Tribenz[b,d,f]azepine-9-yl)propyl)-3-piperidinecarboxylic acid, hydrochloride収率 74.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 14798
Sodium Hydroxide
溶媒

実験手順

The above ester (0.13 g, 0.27 mmol) was dissolved in ethanol (3 ml) and 2N sodium hydroxide (0.6 ml). The mixture was stirred at room temperature for 1.5 hour, acidified by addition of 1N hydrochloric acid (pH 1) and ethanol was removed in vacuo. The aqueous solution was diluted with water (10 ml), washed with diethyl ether (20 ml) and extracted with dichloromethane (30 ml). The organic extract was dried (MgSO4) and concentrated in vacuo to afford 90 mg (74%) of the title compound as a solid.

後処理

  1. customwas removed in vacuo
  2. additionThe aqueous solution was diluted with water (10 ml)
  3. washwashed with diethyl ether (20 ml)
  4. extractionextracted with dichloromethane (30 ml)
  5. extractionThe organic extract
  6. dry with materialwas dried (MgSO4)
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-77571e7262b9455bb2c38e4b470233f3
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05716949

反応ノート

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