1,2-Dichloroethane → HCID 58333391、化合物

HRID 2066843ノート

反応式

HRID 2066843 の反応式
[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([CH2:28][OH:29])=[CH:23][C:22]=3[F:30])[CH2:17][CH2:16]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2].[C:31]([O:35][C:36]([NH:38][CH2:39][C:40](O)=[O:41])=[O:37])([CH3:34])([CH3:33])[CH3:32].C(Cl)CCl.[C+](=O)C1C=CC=CC=1>CN(C1C=CN=CC=1)C.C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:16][CH2:17][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([CH2:28][O:29][C:40](=[O:41])[CH2:39][NH:38][C:36]([O:35][C:31]([CH3:33])([CH3:32])[CH3:34])=[O:37])=[CH:23][C:22]=3[F:30])[CH2:19][CH2:20]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 78288N-(tert-butoxycarbonyl)glycineHCID 5325558HCID 5325558、化合物HCID 58333373HCID 58333373、化合物

生成物 1

HCID 58333391HCID 58333391、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

Compound 10-1 (40 mg, 0.094 mmol), tert-butoxycarbonylamino-acetic acid (17 mg, 0.097 mmol), DMAP (3 mg, 0.024 mmol), EDC(22 mg, 0.11 mmol) and DCM (1 mL) were combined in that order and the reaction mixture was stirred for 20 h. The mixture was then washed with aqueous NaHCO3 (1 mL), concentrated under a stream of nitrogen and purified by Jones flash LC(eluent: 10-40% ethyl acetate+0.1% triethylamine in hexanes) to afford 12-1: LC-MS 408.2 (benzylium fragment).

後処理

  1. washThe mixture was then washed with aqueous NaHCO3 (1 mL)
  2. concentrationconcentrated under a stream of nitrogen
  3. custompurified by Jones flash LC(eluent
  4. custom10-40% ethyl acetate+0.1% triethylamine in hexanes) to afford 12-1

出典と根拠

ORDレコード
ord-123b0e1df30b4c7ab70811e38c746728
出典データセット
uspto-grants-2012_10
特許番号
US08293729B2

反応ノート

読み込み中…