Hydrochloric Acid → HCID 67465156、化合物

HRID 554007ノート

反応式

HRID 554007 の反応式
C1N(P(Cl)(N2C(=O)OCC2)=O)C(=O)OC1.[CH2:16]([O:18][C:19]([CH:21]=[CH:22][CH:23]1[NH:28][CH:27]([C:29]2[CH:34]=[C:33]([F:35])[C:32]([F:36])=[C:31]([F:37])[CH:30]=2)[CH2:26][N:25]([C:38]([O:40][CH3:41])=[O:39])[CH2:24]1)=[O:20])[CH3:17].[CH:42]([CH2:44][C:45](O)=[O:46])=[CH2:43].Cl>C1COCC1.C(OCC)(=O)C.C(N(CC)CC)C>[C:45]([N:28]1[CH:27]([C:29]2[CH:34]=[C:33]([F:35])[C:32]([F:36])=[C:31]([F:37])[CH:30]=2)[CH2:26][N:25]([C:38]([O:40][CH3:41])=[O:39])[CH2:24][CH:23]1[CH:22]=[CH:21][C:19]([O:18][CH2:16][CH3:17])=[O:20])(=[O:46])[CH2:44][CH:42]=[CH2:43]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 327433-Butenoic acidHCID 152842Bis(2-oxo-3-oxazolidinyl)phosphinic chlorideHCID 67464101Methyl 3-(2-ethoxycarbonylvinyl)-5-(3,4,5-trifluorophenyl)piperazine-1-carboxylate

生成物 1

HCID 67465156HCID 67465156、化合物

試薬・触媒・溶媒 3

HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

BOPCl (557 mg) was added to a solution of methyl 3-(2-ethoxycarbonylvinyl)-5-(3,4,5-trifluorophenyl)piperazine-1-carboxylate (422 mg), triethylamine (0.61 mL), and vinylacetic acid (0.19 mL) in THF (15 mL), and the reaction solution was stirred at room temperature for 20 hours. 1 N aqueous hydrochloric acid and ethyl acetate were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with saturated sodium bicarbonate water, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure to obtain 643 mg of an E/Z isomer mixture crude product of the title compound. The property value of the compound is as follows.

後処理

  1. customthe organic layer was separated
  2. washThe resulting organic layer was washed with saturated sodium bicarbonate water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f3b38afad25c4244a2db0e2f777f6d1c
出典データセット
uspto-grants-2011_11
特許番号
US08048878B2

反応ノート

読み込み中…