Cinnamic Acid → (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt

HRID 1464930노트

반응식

HRID 1464930 반응식
[C:1]([OH:11])(=[O:10])/[CH:2]=[CH:3]/[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Cl:12][C:13]1[CH:14]=[CH:15][C:16]2[CH2:22][CH2:21][NH:20][CH2:19][C@H:18]([CH3:23])[C:17]=2[CH:24]=1>C(#N)C>[C:1]([OH:11])(=[O:10])/[CH:2]=[CH:3]/[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.[Cl:12][C:13]1[CH:14]=[CH:15][C:16]2[CH2:22][CH2:21][NH:20][CH2:19][C@H:18]([CH3:23])[C:17]=2[CH:24]=1

참가 물질

4

반응물 2

HCID 444539Cinnamic AcidHCID 11658860Lorcaserin

생성물 1

HCID 56925140(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt was prepared by combining one equivalent of trans-cinnamic acid with (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in acetonitrile at 50° C. The sample was cooled slowly and stirred overnight. The resulting white solid was isolated by filtration and dried. Similar samples prepared in isopropanol, acetone or THF produced white solids only after removal of solvent and trituration with MTBE. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt had an extrapolated melting onset temperature by DSC of 106° C.

후처리

  1. customat 50° C
  2. temperatureThe sample was cooled slowly
  3. customThe resulting white solid was isolated by filtration
  4. customdried
  5. customSimilar samples prepared in isopropanol
  6. customacetone or THF produced white solids only after removal of solvent and trituration with MTBE
  7. customby DSC of 106° C.

출처 및 근거

ORD 기록
ord-ab93591aca7e4ddfbcd87ff0ad28080b
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999970B2

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