Tetrahydrofuran → HCID 86676230、化合物

HRID 1409081ノート

反応式

HRID 1409081 の反応式
[C:1]([O:5][C:6]([N:8]([CH2:17][CH:18]=[CH2:19])[CH:9]([CH2:14][CH:15]=[CH2:16])[C:10](OC)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].O1CCCC1.[H-].C([Al+]CC(C)C)C(C)C.C1(C)C=CC=CC=1>C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>[OH:11][CH2:10][CH:9]([N:8]([CH2:17][CH:18]=[CH2:19])[C:6](=[O:7])[O:5][C:1]([CH3:2])([CH3:3])[CH3:4])[CH2:14][CH:15]=[CH2:16]

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 11108397Methyl 2-[[(1,1-dimethylethoxy)carbonyl]-2-propen-1-ylamino]-4-pentenoateHCID 86583787Diisobutylaluminumhydride toluene

生成物 1

HCID 86676230HCID 86676230、化合物収率 83.9%

試薬・触媒・溶媒 1

HCID 9855836Potassium sodium tartarate溶媒

実験手順

To a mixture of methyl 2-[(tert-butoxycarbonyl) (prop-2-en-1-yl)amino]pent-4-enoate (5.0 g) produced above and tetrahydrofuran (100 mL) was added 1M diisobutylaluminum hydride/toluene solution (60 mL) at 0° C., and the mixture was stirred at the same temperature for 15 min. The reaction mixture was diluted with aqueous potassium sodium tartrate solution, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate. Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure to give the title compound (3.76 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. filtrationInsoluble material was filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-a75340f2599d47b5a42ef66578718a72
出典データセット
uspto-grants-2014_12
特許番号
US08921354B2

反応ノート

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