1,8-Diazabicyclo(5.4.0)undec-7-ene → 1055306-64-3

HRID 1426689ノート

反応式

HRID 1426689 の反応式
Br[CH2:2][CH:3]1[CH2:7][N:6]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[C:5](=[O:15])[C:4]1([F:17])[F:16].N12CCCN=C1CCCCC2>O1CCCC1>[F:17][C:4]1([F:16])[C:3](=[CH2:2])[CH2:7][N:6]([C:8]([O:10][C:11]([CH3:12])([CH3:14])[CH3:13])=[O:9])[C:5]1=[O:15]

参加物

4

反応物 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 59826883Tert-butyl 4-(bromomethyl)-3,3-difluoro-2-oxopyrrolidine-1-carboxylate

生成物 1

HCID 598268761055306-64-3収率 76%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of tert-butyl 4-(bromomethyl)-3,3-difluoro-2-oxopyrrolidine-1-carboxylate (50.1 g) in tetrahydrofuran (400 mL) was added dropwise 1,8-diazabicyclo[5.4.0]undec-7-ene (25.0 mL) at 0° C. over 15 min. After the completion of the dropwise addition, the mixture was stirred at room temperature for 1 hr. Insoluble materials were filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=4:1). The obtained crystals were washed with diisopropyl ether to give the title compound as colorless crystals (yield 28.1 g, 76%).

後処理

  1. additionAfter the completion of the dropwise addition
  2. filtrationInsoluble materials were filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=4:1)
  5. washThe obtained crystals were washed with diisopropyl ether

出典と根拠

ORDレコード
ord-67447c9b1604489a8606fe3d57a37ccc
出典データセット
uspto-grants-2015_01
特許番号
US08933105B2

反応ノート

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