反応 #1552116

ord-748eab108e5e454b8e6abfb7448b8270

反応方程式

O=C1CC[C@@H](C(=O)O)N1
pyroglutamic acid
C[C@H]1CNCCc2ccc(Cl)cc21
(R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine
C[C@H]1CNCCc2ccc(Cl)cc21.O=C1CC[C@@H](C(=O)O)N1
(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine pyroglutamate salt

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他at 60° C.
  2. 2
    温度then cooling slowly
  3. 3
    その他The resulting white solid was isolated by filtration
  4. 4
    その他dried
  5. 5
    その他by DSC of about 139° C.

実験手順

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine pyroglutamate salt was prepared by combining one equivalent of pyroglutamic acid with (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in ethyl acetate at 60° C. then cooling slowly and stirring overnight. The resulting white solid was isolated by filtration and dried. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine pyroglutamate salt had an extrapolated melting onset temperature by DSC of about 139° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08999970B2uspto-grants-2015_04