1-Butanol → 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one

HRID 267779

反応式

HRID 267779 の反応式
[OH:1][C:2]1([CH2:13][NH:14][CH:15]([CH3:17])[CH3:16])[CH2:8][O:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[O:4][CH2:3]1.[C:18](=O)(OCCCC)[O:19]CCCC.[Na].C(O)CCC>C1C=CC=CC=1>[CH:15]([N:14]1[CH2:13][C:2]2([CH2:8][O:7][C:6]3[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=3[O:4][CH2:3]2)[O:1][C:18]1=[O:19])([CH3:17])[CH3:16]

参加物

6

反応物 4

HCID 2631-ButanolHCID 68333Dibutyl carbonate2 回HCID 5360545SodiumHCID 15557308HCID 15557308、化合物

生成物 1

HCID 155573263'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 3-hydroxy-3-isopropylaminomethyl-3,4-dihydro-2H-1,5-benzodioxepin (11.85 g.; 50 millimoles), prepared as described in Example 1, and dibutyl carbonate (13.1 g.) with a small piece of metallic sodium is heated in an oil bath. The temperature then is slowly raised to 170° C. with removal of butanol. Finally, the mixture is heated between 170°-200° C. with removal of excess dibutyl carbonate. The cooled reaction product is dissolved in benzene, washed with water, dried over sodium sulfate, and the solvent evaporated to give 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one, m.p. 121°-122° C.

後処理

  1. customprepared
  2. temperatureis heated in an oil bath
  3. customThe cooled reaction product
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customthe solvent evaporated

出典と根拠

ORDレコード
ord-baf10c7490ea425cbcdd0e469640b157
出典データセット
uspto-grants-1976_03
特許番号
US03944560

関連ノート

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