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Hydrochloric Acid → Atomoxetine Hydrochloride

HRID 2099918
ノート
印刷プレビュー

反応式

HRID 2099918 の反応式
[ClH:1].[CH3:2][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:8]=1[O:9][C@@H:10]([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)[CH2:11][CH2:12][NH:13][CH3:14]>C(OCCCC)(=O)C>[CH3:2][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:8]=1[O:9][C@@H:10]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:11][CH2:12][NH:13][CH3:14].[ClH:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 54841Atomoxetine

生成物 1

HCID 54840Atomoxetine Hydrochloride収率 122.4%

試薬・触媒・溶媒 1

HCID 31272Butyl Acetate溶媒

実験手順

Under stirring, while maintaining the temperature between about 22° C. and about 25° C. with a water bath, 286 g (2.825 mol) of aqueous hydrogen chloride (36%) are dropped on 5063 g (2.379 mol) of Atomoxetine base in a solution of n-butyl acetate, prepared as described in U.S. Provisional Applications Nos. 60/583643, 60/583644, and 60/622065. The hydrochloride crystallized. The resulting suspension is stirred at about 25° C. for about one hour, and the solid is collected by filtration, and washed three times with 900 ml of n-butyl acetate. About 850 g of wet Atomoxetine Hydrochloride are obtained. After two separate preparations, samples of obtained wet solids are dissolved in water (2 g in 100 ml). The pH determined for each sample is 2.39 and pH 2.40, respectively.

後処理

  1. temperaturewhile maintaining the temperature between about 22° C. and about 25° C. with a water bath
  2. customprepared
  3. customThe hydrochloride crystallized
  4. stirringThe resulting suspension is stirred at about 25° C. for about one hour
  5. filtrationthe solid is collected by filtration
  6. washwashed three times with 900 ml of n-butyl acetate

出典と根拠

ORDレコード
ord-09ffef65b06c448195a3b65d6e54f90f
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07569729B2

反応ノート

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