Hydrochloric Acid → (S)-(3-(Azetidin-3-ylamino)pyrrolidin-1-yl)(phenyl)methanone

HRID 403287ノート

反応式

HRID 403287 の反応式
C(OC([N:8]1[CH2:11][CH:10]([NH:12][C@H:13]2[CH2:17][CH2:16][N:15]([C:18](=[O:25])[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14]2)[CH2:9]1)=O)(C)(C)C.Cl>CO.O1CCOCC1>[NH:8]1[CH2:9][CH:10]([NH:12][C@H:13]2[CH2:17][CH2:16][N:15]([C:18]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:25])[CH2:14]2)[CH2:11]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 67288181(S)-tert-Butyl-3-((1-benzoylpyrrolidin-3-yl)amino)azetidine-1-carboxylate

生成物 1

HCID 67288563(S)-(3-(Azetidin-3-ylamino)pyrrolidin-1-yl)(phenyl)methanone

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of compound 5d (0.96 g, 2.78 mmol) in MeOH (5 mL) was added HCl solution in dioxane (4M, 10 mL) at room temperature. The mixture was stirred at room temperature for 4 h. The solvent was removed by evaporation. Ether (50 mL) was added to the residue. The off-white solid was collected by filtration, washed with hexanes, and dried under vacuum. The crude compound 5e was used in the next reaction without further purification. MS m/z (M+H+) 246.0.

後処理

  1. customThe solvent was removed by evaporation
  2. additionEther (50 mL) was added to the residue
  3. filtrationThe off-white solid was collected by filtration
  4. washwashed with hexanes
  5. customdried under vacuum
  6. customThe crude compound 5e was used in the next reaction without further purification

出典と根拠

ORDレコード
ord-60b883c7bd42414d99cde428f4ad3807
出典データセット
uspto-grants-2014_06
特許番号
US08748417B2

反応ノート

読み込み中…