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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 67025190、化合物

HRID 1512734
ノート
印刷プレビュー

反応式

HRID 1512734 の反応式
CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[C:22]([C:24]1[CH:25]=[C:26]([CH:30]=[CH:31][C:32]=1[O:33][CH:34]([CH3:36])[CH3:35])[C:27]([OH:29])=O)#[N:23].O[NH:38][C:39](=[NH:58])[C:40]1[CH:48]=[C:47]2[C:43]([C:44]([CH2:49][CH2:50][C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])=[CH:45][NH:46]2)=[CH:42][CH:41]=1>CN(C=O)C>[C:22]([C:24]1[CH:25]=[C:26]([C:27]2[O:29][N:38]=[C:39]([C:40]3[CH:48]=[C:47]4[C:43]([C:44]([CH2:49][CH2:50][C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])=[CH:45][NH:46]4)=[CH:42][CH:41]=3)[N:58]=2)[CH:30]=[CH:31][C:32]=1[O:33][CH:34]([CH3:36])[CH3:35])#[N:23]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 21956832RP-101124HCID 178450933HCID 178450933、化合物

生成物 1

HCID 67025190HCID 67025190、化合物収率 33.9%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
80 °C

実験手順

EDCI (151 mg) and HOBT (121 mg) were added to a solution of 3-cyano-4-[(1-methylethyl)oxy]benzoic acid (can be prepared as described in WO2005/58848, 135 mg) in DMF (5 mL) at RT. The resulting solution was stirred for 45 min. 1,1-dimethylethyl 3-{6-[(hydroxyamino)(imino)methyl]-1H-indol-3-yl}propanoate (D16) (199 mg) was added and the reaction mixture was stirred at RT for 3 hours. The reaction mixture was heated to 80° C. and stirred at that temperature for 5 hours. DMF was evaporated. EtOAc (100 mL) was added and the organic solution was washed with saturated aqueous sodium bicarbonate solution (75 mL) and water (75 mL). The organic fraction was dried over anhydrous magnesium sulfate. The dried solution was concentrated. The residue was purified by Biotage (25→33% EtOAc in hexane) to afford 1,1-dimethylethyl 3-[6-(5-{3-cyano-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indol-3-yl]propanoate (D19) (105 mg) as a white solid. δH (DMSO-d6, 400 MHz): 1.38 (9H, s), 1.39 (6H, d), 2.60 (2H, t), 2.96 (2H, t), 4.98 (1H, m), 7.35 (1H, d), 7.55 (1H, d), 7.72 (2H, m), 8.12 (1H, d), 8.42 (1H, dd), 8.51 (1H, d), 11.21 (1H, s). MS (ES): C27H28N4O4 requires 472; found 473.0 (M+H+).

後処理

  1. stirringthe reaction mixture was stirred at RT for 3 hours
  2. stirringstirred at that temperature for 5 hours
  3. customDMF was evaporated
  4. additionEtOAc (100 mL) was added
  5. washthe organic solution was washed with saturated aqueous sodium bicarbonate solution (75 mL) and water (75 mL)
  6. dry with materialThe organic fraction was dried over anhydrous magnesium sulfate
  7. concentrationThe dried solution was concentrated
  8. customThe residue was purified by Biotage (25→33% EtOAc in hexane)

出典と根拠

ORDレコード
ord-d772084cf801483dba4576617f8db2fb
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217028B2

反応ノート

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