Methyl morpholine oxide → HCID 19611677、化合物

HRID 1602380ノート

反応式

HRID 1602380 の反応式
C[N+]1([O-])CC[O:5]CC1.Br[CH2:10][C:11]1[C:16]2[CH:17]=[CH:18][O:19][C:15]=2[C:14]([Cl:20])=[CH:13][CH:12]=1>C(#N)C>[Cl:20][C:14]1[CH:13]=[CH:12][C:11]([CH:10]=[O:5])=[C:16]2[C:15]=1[O:19][CH:18]=[CH:17]2

参加物

4

反応物 2

HCID 82029Methyl morpholine oxideHCID 19611696HCID 19611696、化合物

生成物 1

HCID 19611677HCID 19611677、化合物収率 73.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of the N-methylmorpholine-N-oxide (37.64 g) in aoetonitrile (370 ml) containing 3 Å molecular sieves (36.6 g) was stirred at room temperature overnight and cooled in ice. A solution of 4-bromomethyl-7-chloro-benzofuran (39.44 g) in acetonitrile (90 ml) was added and the mixture stirred in at 0° C. for 4 h. The mixture was filtered and the filtrate evaporated to dryness. Water and ethyl acetate were added to the residue and the organic phase separated, dried (Na2SO4) and evaporated to give the title compound (21.3 g) as a pale yellow solid.

後処理

  1. temperaturecooled in ice
  2. stirringthe mixture stirred in at 0° C. for 4 h
  3. filtrationThe mixture was filtered
  4. customthe filtrate evaporated to dryness
  5. additionWater and ethyl acetate were added to the residue
  6. customthe organic phase separated
  7. dry with materialdried (Na2SO4)
  8. customevaporated

出典と根拠

ORDレコード
ord-e3b7f707ab4d4a74beb84622911d5f84
出典データセット
uspto-grants-1999_11
特許番号
US05981572

反応ノート

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