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Acetic Acid → Amrubicin Hydrochloride

HRID 842584
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HRID 842584 반응식
[ClH:1].C(O)(=O)C.[CH3:6][C:7]([C@@:9]1([NH2:40])[CH2:30][C@H:29]([O:31][C@@H:32]2[O:37][CH2:36][C@@H:35]([OH:38])[C@@H:34]([OH:39])[CH2:33]2)[C:12]2[C:13]([OH:28])=[C:14]3[C:26](=[O:27])[C:25]4[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=4[C:18](=[O:19])[C:15]3=[C:16]([OH:17])[C:11]=2[CH2:10]1)=[O:8].CC(C)=O>O>[CH3:6][C:7]([C@@:9]1([NH2:40])[CH2:30][C@H:29]([O:31][C@@H:32]2[O:37][CH2:36][C@@H:35]([OH:38])[C@@H:34]([OH:39])[CH2:33]2)[C:12]2[C:13]([OH:28])=[C:14]3[C:26](=[O:27])[C:25]4[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=4[C:18](=[O:19])[C:15]3=[C:16]([OH:17])[C:11]=2[CH2:10]1)=[O:8].[ClH:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 180Acetone2회HCID 313Hydrochloric AcidHCID 3035016Amrubicin

생성물 1

HCID 114897Amrubicin Hydrochloride

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1N Hydrochloric acid (2.05 g) and acetic acid (0.75 g) were added to a solution of amrubicin (1.0 g) in water (10 g) and acetone (6.7 g) at 0 to 5° C., to adjust the pH to 2.5, and stirred for 30 minutes. The reaction mixture was poured into acetone (280 g) at 30 to 34° C., and stirred for 3 hours. The precipitated crystals were collected by filtration, and washed with acetone (9.8 g) to give wet crystals of amrubicin hydrochloride. The wet crystals were added again to mixture of acetone (280 g) and water (11.8 g), and stirred at 30 to 34° C. for 1 hour. The crystals were collected by filtration, and washed with acetone (9.8 g), and dried under reduced pressure at room temperature.

후처리

  1. stirringstirred for 3 hours
  2. filtrationThe precipitated crystals were collected by filtration
  3. washwashed with acetone (9.8 g)

출처 및 근거

ORD 기록
ord-73f69293d9c644b2b58d41baf56e2a51
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06376469B1

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