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Hydrochloric Acid → HCID 9933004, 화합물

HRID 962365
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HRID 962365 반응식
[NH:1]([CH2:16][CH:17]([CH:19]1[CH2:24][CH2:23][C:22]2[CH:25]=[C:26]([F:29])[CH:27]=[CH:28][C:21]=2[O:20]1)[OH:18])[CH2:2][CH:3]([CH:5]1[CH2:10][CH2:9][C:8]2[CH:11]=[C:12]([F:15])[CH:13]=[CH:14][C:7]=2[O:6]1)[OH:4].[ClH:30]>C(O)C>[ClH:30].[NH:1]([CH2:16][CH:17]([CH:19]1[CH2:24][CH2:23][C:22]2[CH:25]=[C:26]([F:29])[CH:27]=[CH:28][C:21]=2[O:20]1)[OH:18])[CH2:2][CH:3]([CH:5]1[CH2:10][CH2:9][C:8]2[CH:11]=[C:12]([F:15])[CH:13]=[CH:14][C:7]=2[O:6]1)[OH:4]
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

(±)-[2R*[1S*,5S*(S*)]]+[2R*[1S*,5R*(R*)]]-α,α'[iminobis(methylene)]bis[6-fluoro-3,4-dihydro-2H-1-benzopyran-2-methanol] (142 g) was converted into the hydrochloric acid salt in ethanol (1000 ml). The crystals were filtered off and crystallized from ethanol. The second fraction of the crystallization was recrystallized from ethanol, yielding 10.3 g (6.6%) of (±)-[2R*[1S*,5S*(S*)]]-α,α'[iminobis(methylene)]bis[6-fluoro-3,4-dihydro-2H-1-benzopyran-2-methanol]hydrochloride; mp. 224.9° C. nebivolol hydrochloride (crystalline compound 1).

후처리

  • filtrationThe crystals were filtered off
  • customcrystallized from ethanol
  • customThe second fraction of the crystallization
  • customwas recrystallized from ethanol
  • 출처 및 근거

    ORD 기록
    ord-65b8cf1f5b3045fb855b479b47c7a633
    출처 데이터셋
    uspto-grants-1998_06
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05759580

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