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Hydrochloric Acid → HCID 9933004、化合物

HRID 451585
ノート
印刷プレビュー

反応式

HRID 451585 の反応式
[CH:1]1[C:6]([F:7])=[CH:5][C:4]2[CH2:8][CH2:9][CH:10]([CH:12]([OH:29])[CH2:13][NH:14][CH2:15][CH:16]([OH:28])[CH:17]3[O:26][C:25]4[CH:24]=[CH:23][C:22]([F:27])=[CH:21][C:20]=4[CH2:19][CH2:18]3)[O:11][C:3]=2[CH:2]=1.[ClH:30]>C(O)C>[CH:23]1[C:22]([F:27])=[CH:21][C:20]2[CH2:19][CH2:18][CH:17]([CH:16]([OH:28])[CH2:15][NH:14][CH2:13][CH:12]([OH:29])[CH:10]3[O:11][C:3]4[CH:2]=[CH:1][C:6]([F:7])=[CH:5][C:4]=4[CH2:8][CH2:9]3)[O:26][C:25]=2[CH:24]=1.[ClH:30]
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 71301Nebivolol

生成物 1

HCID 9933004HCID 9933004、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Nebivolol free base (3.30 g, 8.70 mmol) is suspended in absolute ethanol (100 mL) and heated to fall until complete dissolution. To this solution, 1.25 M ethanolic HCl (7.5 mL) is added. The obtained solution is concentrated under reduced pressure, until obtaining a 15% concentration of the product. During solvent evaporation, progressive formation of a white precipitate is observed. The solid is filtered by washing with cold absolute ethanol, to obtain 3.10 g of nebivolol hydrochloride salt. The chiral purity of the product and the ratio between the two enantiomers is evaluated by comparison with reference standards, by HPLC with an AKZO NOBEL column, Kromasil 5-AmyCoat, 5 μm, 250 mm×4.6 and a suitable binary gradient.

後処理

  1. temperatureheated
  2. dissolutionto fall until complete dissolution
  3. concentrationThe obtained solution is concentrated under reduced pressure
  4. customuntil obtaining a 15% concentration of the product
  5. customDuring solvent evaporation, progressive formation of a white precipitate
  6. filtrationThe solid is filtered
  7. washby washing with cold absolute ethanol

出典と根拠

ORDレコード
ord-527305b698b341f4936fa7e3e7732e29
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08487122B2

反応ノート

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