Sodium borohydride → HCID 14580514、化合物

HRID 1613610ノート

反応式

HRID 1613610 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:13][CH2:12][CH2:11][CH2:10][C:9](=[O:14])[C:8]=2[CH:15]=1)([O-:3])=[O:2].[BH4-].[Na+]>CO>[OH:14][CH:9]1[C:8]2[CH:15]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=[CH:6][C:7]=2[O:13][CH2:12][CH2:11][CH2:10]1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 145805137-Nitro-3,4-dihydro-1-benzoxepin-5(2H)-one

生成物 1

HCID 14580514HCID 14580514、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

32.1 g (0.155 mole) of 2,3-dihydro-7-nitro-1-benzoxepin-5(4H)-one are suspended in 220 ml of methanol and, while stirring at 0° C. under argon, 6.5 g (0.17 mole) of sodium borohydride are added in portions. The mixture is then stirred for about 30 minutes and stirred into ice/water, and the precipitated solid is filtered off with suction and thoroughly washed with water. The solid is taken up in the ethyl acetate, and the solution is separated from the water, dried over sodium sulfate, filtered and evaporated in vacuo. The residue is crystallized in diisopropyl ether/cyclohexane with the addition of active charcoal.

後処理

  1. stirringThe mixture is then stirred for about 30 minutes
  2. filtrationthe precipitated solid is filtered off with suction
  3. washthoroughly washed with water
  4. customthe solution is separated from the water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. customThe residue is crystallized in diisopropyl ether/cyclohexane with the addition of active charcoal

出典と根拠

ORDレコード
ord-9f5aaf09d62047598bd46e105bfaee75
出典データセット
uspto-grants-1993_03
特許番号
US05194442

反応ノート

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