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Maleic Acid → HCID 86659301, 화합물

HRID 1911811
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HRID 1911811 반응식
[NH:1]1[CH2:5][CH2:4][C@H:3](/[CH:6]=[CH:7]/[C:8]2[CH:9]=[N:10][CH:11]=[N:12][CH:13]=2)[CH2:2]1.[C:14]([OH:21])(=[O:20])/[CH:15]=[CH:16]\[C:17]([OH:19])=[O:18]>C(#N)C>[C:14]([OH:21])(=[O:20])/[CH:15]=[CH:16]\[C:17]([OH:19])=[O:18].[NH:1]1[CH2:5][CH2:4][C@H:3](/[CH:6]=[CH:7]/[C:8]2[CH:13]=[N:12][CH:11]=[N:10][CH:9]=2)[CH2:2]1
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참가 물질

4

반응물 2

HCID 444266Maleic AcidHCID 11528435Simpinicline

생성물 1

HCID 86659301HCID 86659301, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
50 °C

실험 절차

(R)-5-((E)-2-pyrrolidin-3-ylvinyl)pyrimidine free base (189 mg, 1.077 mmol, freshly prepared) was dissolved in acetonitrile (5 ml). The solution was then treated with 1.1 eq. of an maleic acid solution (1M in tetrahydrofuran) at ambient temperature. The mixture was warmed up to 50° C. and cooled down slowly to ambient temperature overnight. The solid obtained was filtered and dried under suction before being analysed by XRPD, and 1H-NMR. The XRPD diffractogram of (R)-5-((E)-2-pyrrolidin-3-ylvinyl)pyrimidine mono-maleate Form I is shown in FIG. 7.

후처리

  1. temperaturecooled down slowly to ambient temperature overnight
  2. customThe solid obtained
  3. filtrationwas filtered
  4. customdried under suction

출처 및 근거

ORD 기록
ord-1f4b2641f0c44647b10886ff06a30f59
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08604191B2

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