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Hydrochloric Acid → HCID 9933004, 화합물

HRID 451585
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HRID 451585 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 71301Nebivolol

생성물 1

HCID 9933004HCID 9933004, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-527305b698b341f4936fa7e3e7732e29
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08487122B2

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