Ethanol → 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol L-tartrate

HRID 2377165

반응식

HRID 2377165 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][CH2:15][N:16]3[CH2:19][CH:18]([OH:20])[CH2:17]3)=[CH:9][C:4]=2[CH:3]=[CH:2]1.[C:21]([OH:30])(=[O:29])[C@@H:22]([C@H:24]([C:26]([OH:28])=[O:27])[OH:25])[OH:23].C(O)C>C(OCC)(=O)C>[C:26]([C@@H:24]([C@H:22]([C:21]([OH:30])=[O:29])[OH:23])[OH:25])([OH:28])=[O:27].[S:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][CH2:15][N:16]3[CH2:19][CH:18]([OH:20])[CH2:17]3)=[CH:9][C:4]=2[CH:3]=[CH:2]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 444305L-Tartaric acidHCID 9901946Edonerpic

생성물 1

HCID 665884561-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol L-tartrate수율 91.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

반응 조건

온도
65 °C

실험 절차

In 40 mL of ethyl acetate was dissolved 10.0 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol, and 5.15 g of L-tartaric acid and 40 mL of ethanol were added thereto, after which the resulting mixture was heated at 65° C. to effect dissolution. After the resulting solution was stirred at 50° C. for 20 minutes, 40 mL of ethyl acetate was added dropwise thereto at the same temperature and the resulting mixture was stirred at 20 to 30° C. for 1 hour. The crystals precipitated were collected by filtration to obtain 13.9 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol L-tartrate as colorless crystals.

후처리

  1. additionwere added
  2. dissolutiondissolution
  3. stirringat the same temperature and the resulting mixture was stirred at 20 to 30° C. for 1 hour
  4. customThe crystals precipitated
  5. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-5d163b3710d146edb53cebe3b854e2a4
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07468443B2

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