1,5-Dibromopentane → 6-(5-bromopentoxy)-4,4-dimethyl-4H-3,1-benzoxazin-2-one

HRID 463061노트

반응식

HRID 463061 반응식
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:10][C:9](=[O:11])[O:8][C:7]([CH3:13])([CH3:12])[C:6]=2[CH:14]=1.C(=O)([O-])[O-].[K+].[K+].[Br:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]Br>CS(C)=O>[Br:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][O:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:10][C:9](=[O:11])[O:8][C:7]([CH3:12])([CH3:13])[C:6]=2[CH:14]=1

참가 물질

5

반응물 3

HCID 81001,5-DibromopentaneHCID 11430Potassium CarbonateHCID 132604826-hydroxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one

생성물 1

HCID 132604896-(5-bromopentoxy)-4,4-dimethyl-4H-3,1-benzoxazin-2-one

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A solution of 19.3 gm (0.1 mol) of 6-hydroxy-4,4-dimethyl-4H-3,1-benzoxazin-2-one in 200 ml of dimethyl sulfoxide is mixed at ambient temperature with 41.5 gm (0.3 mol) of potassium carbonate and 92 gm (0.4 mol) of 1,5-dibromopentane, whereupon the temperature rises to 45° C. After stirring a further two hours, ice water is added, and the resulting mixture is extracted with chloroform. The chloroform phase is washed with water and dried with sodium sulfate, and the chloroform is distilled off. The residue is recrystallized from ethyl acetate/petroleum ether.

후처리

  1. customrises to 45° C
  2. extractionthe resulting mixture is extracted with chloroform
  3. washThe chloroform phase is washed with water
  4. dry with materialdried with sodium sulfate
  5. distillationthe chloroform is distilled off
  6. customThe residue is recrystallized from ethyl acetate/petroleum ether

출처 및 근거

ORD 기록
ord-94624531fa3a40dbbf91beb17f72f0b4
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04518597

반응 노트

불러오는 중…