Sodium hydride → 4-Benzyl-7,7-diphenyl-1,4-oxazepan-3-one

HRID 596164ノート

反応式

HRID 596164 の反応式
[CH2:1]([N:8]([CH2:13][CH2:14][C:15]([OH:28])([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:9](=[O:12])[CH2:10]Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+]>CN(C)C=O>[CH2:1]([N:8]1[CH2:13][CH2:14][C:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[O:28][CH2:10][C:9]1=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24758Sodium hydrideHCID 20326654N-benzyl-N-chloroacetyl-3hydroxy-3,3-diphenylpropylamine

生成物 1

HCID 203266404-Benzyl-7,7-diphenyl-1,4-oxazepan-3-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

The solution of 19.3 g of N-benzyl-N-chloroacetyl-3hydroxy-3,3-diphenylpropylamine in 150 ml of dimethylformamide is added dropwise to the suspension of 1.2 g of sodium hydride in 50 ml of dimethylformamide while stirring and cooling with an ice-bath. The mixture is allowed to warm up to room temperature, stirred for 15 hours and evaporated. The residue is partitioned between 150 ml methylene chloride and 50 ml of N hydrochloric acid, the organic layer separated, washed with water, dried, filtered and evaporated. The residue is triturated with diethyl ether and recrystallized from ethanol, to yield the 4-benzyl-3-oxo-7,7-diphenyl-hexahydro-1,4-oxazepine of the formula ##STR7## melting at 185° to 186°.

後処理

  1. temperaturecooling with an ice-bath
  2. stirringstirred for 15 hours
  3. customevaporated
  4. customThe residue is partitioned between 150 ml methylene chloride and 50 ml of N hydrochloric acid
  5. customthe organic layer separated
  6. washwashed with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue is triturated with diethyl ether
  11. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-220e732c0ebe466ebed9812668e1f5d2
出典データセット
uspto-grants-1977_03
特許番号
US04010166

反応ノート

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