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

HRID 463061ノート

反応式

HRID 463061 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94624531fa3a40dbbf91beb17f72f0b4
出典データセット
uspto-grants-1985_05
特許番号
US04518597

反応ノート

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