Sodium Carbonate → HCID 13446113、化合物

HRID 1277929ノート

反応式

HRID 1277929 の反応式
[BH4-].[Na+].[CH3:3][NH:4][C:5]1[CH2:6][O:7][C:8]2[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=2[C:10](=[O:12])[CH:11]=1.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1.C(O)(=O)C>[CH3:3][NH:4][CH:5]1[CH2:11][CH:10]([OH:12])[C:9]2[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=2[O:7][CH2:6]1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 4311764Sodium borohydride2 回HCID 134460473-(Methylamino)-1-benzoxepin-5(2H)-one

生成物 1

HCID 13446113HCID 13446113、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

Sodium borohydride is added in small portions to a solution of 18.8 g (0.1 mole) 3-methylamino-1-benzoxepin-5-(2H)-one in a mixture of 125 ml dioxane and 125 ml acetic acid cooled in an ice bath. The reaction solution is maintained in a cooled state during the addition of the sodium borohydride (0.4 mole) up to the end of the reaction. The reaction solution is then poured into ice water, made alkaline with sodium carbonate and extracted with dichloromethane. The organic solution is washed with saturated salt solution and dried over sodium sulfate. After removal of the solvent, 16.4 g (85% of the theoretical yield) of racemic-2,3,4,5-tetrahydro-3-methylamino-1-benzoxepin-5-ol is recovered in the form of an oil.

後処理

  1. temperaturecooled in an ice bath
  2. extractionextracted with dichloromethane
  3. washThe organic solution is washed with saturated salt solution
  4. dry with materialdried over sodium sulfate
  5. customAfter removal of the solvent, 16.4 g (85% of the

出典と根拠

ORDレコード
ord-31c7455639ee4d86a48beee68e931064
出典データセット
uspto-grants-1981_07
特許番号
US04279904

反応ノート

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