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

HRID 267779노트

반응식

HRID 267779 반응식
[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]

참가 물질

6

반응물 4

HCID 2631-ButanolHCID 68333Dibutyl carbonate2회HCID 5360545SodiumHCID 15557308HCID 15557308, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-baf10c7490ea425cbcdd0e469640b157
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03944560

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