Hydrochloric Acid → 1'-(4-phenoxybenzoyl)-1,3'-bipyrrolidine Hydrochloride

HRID 1176055ノート

反応式

HRID 1176055 の反応式
[ClH:1].[N:2]1([CH:7]2[CH2:11][CH2:10][NH:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3]1.[O:12]([C:19]1[CH:27]=[CH:26][C:22]([C:23](O)=[O:24])=[CH:21][CH:20]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.F[P-](F)(F)(F)(F)F.N1(O[P+](N2CCCC2)(N2CCCC2)N2CCCC2)C2C=CC=CC=2N=N1>C(Cl)Cl.C(N(CC)CC)C>[ClH:1].[O:12]([C:19]1[CH:20]=[CH:21][C:22]([C:23]([N:9]2[CH2:10][CH2:11][CH:7]([N:2]3[CH2:6][CH2:5][CH2:4][CH2:3]3)[CH2:8]2)=[O:24])=[CH:26][CH:27]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 751824-Phenoxybenzoic acidHCID 2724699PyBOPHCID 146273751-(Pyrrolidin-3-yl)pyrrolidine

生成物 1

HCID 684299591'-(4-phenoxybenzoyl)-1,3'-bipyrrolidine Hydrochloride

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine溶媒

実験手順

A stirred mixture of the HCl salt of 3-(pyrrolidino)pyrrolidine (0.44 g, 2.1 mmol) and 4-phenoxy benzoic acid (0.34 g, 1.6 mmol) in CH2Cl2 is treated with 0.85 mL of triethylamine at room temperature. The reaction mixture is treated with solid benzotriazol-1-yl-oxytripyrrolidinophosphonium hexafluorophosphate (1.2 g, 2.4 mmol), stirred overnight under nitrogen, diluted with CH2Cl2, washed sequentially with water and brine, dried over MgSO4 and concentrated in vacuo. The resultant residue is chromatographed and treated with HCl in ether to afford the title compound as a white solid, identified by NMR and MS analyses.

後処理

  1. washwashed sequentially with water and brine
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe resultant residue is chromatographed
  5. additiontreated with HCl in ether

出典と根拠

ORDレコード
ord-305a18e88c974a8c85b72b7464061ecf
出典データセット
uspto-grants-2010_11
特許番号
US07842715B2

反応ノート

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