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Nitrogen → t-Butyl-2-methacryloyloxyacetate

HRID 7337
ノート
印刷プレビュー

反応式

HRID 7337 の反応式
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].Br[CH2:8][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10].C1CCN2C(=NCCC2)CC1.N#N>C1(C)C=CC=CC=1>[C:12]([O:11][C:9](=[O:10])[CH2:8][O:5][C:1](=[O:6])[C:2]([CH3:4])=[CH2:3])([CH3:15])([CH3:14])[CH3:13]
参加物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 947NitrogenHCID 4093Methacrylic AcidHCID 79177tert-Butyl bromoacetateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene

生成物 1

HCID 14958425t-Butyl-2-methacryloyloxyacetate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Methacrylic acid (8.06 g, 0.10 mole), t-butyl bromoacetate (19.50 g, 0.10 mole) and 1,8-diazabicyclo[5.4.0]undoc-7-ene, DBU, (15.20 g, 0.10 mole) and 150 ml toluene were combined in a 500 ml 3-neck flask equipped with condenser, nitrogen inlet, thermometer and magnetic stirrer bar. The reaction mixture was stirred at room temperature for one hour. The reaction was continued at 90° C. overnight under a blanket of N2 flow. The mixture was cooled to room temperature and the salt was removed by filtration. The toluene solution was washed with 75 ml saturated NaCl solution and 2×75 ml Dl-water respectively before dried on MgSO4 overnight. The solid was filtered out and the toluene was removed at rotavap. An oily residue was distilled to a final clear liquid at reduced pressure.

後処理

  1. customequipped with condenser, nitrogen inlet
  2. temperatureThe mixture was cooled to room temperature
  3. customthe salt was removed by filtration
  4. washThe toluene solution was washed with 75 ml saturated NaCl solution and 2×75 ml Dl-water respectively
  5. custombefore dried on MgSO4 overnight
  6. filtrationThe solid was filtered out
  7. customthe toluene was removed at rotavap
  8. distillationAn oily residue was distilled to a final clear liquid at reduced pressure

出典と根拠

ORDレコード
ord-f9a41ba85d96457aa547e1997e89c67d
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07087356B2

反応ノート

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