Potassium Carbonate → 6-[4-(3,4-Dichloro-phenylsulfinyl)-butoxy]-4,4-dimethyl-4H-3,1-benzoxazin-2-one

HRID 463072ノート

反応式

HRID 463072 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.[Cl:15][C:16]1[CH:17]=[C:18]([S:23]([CH2:25][CH2:26][CH2:27][CH2:28]Br)=[O:24])[CH:19]=[CH:20][C:21]=1[Cl:22].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[Cl:15][C:16]1[CH:17]=[C:18]([S:23]([CH2:25][CH2:26][CH2:27][CH2:28][O:1][C:2]2[CH:3]=[CH:4][C:5]3[NH:10][C:9](=[O:11])[O:8][C:7]([CH3:12])([CH3:13])[C:6]=3[CH:14]=2)=[O:24])[CH:19]=[CH:20][C:21]=1[Cl:22]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 130846014-(4-Bromobutane-1-sulfinyl)-1,2-dichlorobenzeneHCID 132604826-hydroxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one

生成物 1

HCID 132539416-[4-(3,4-Dichloro-phenylsulfinyl)-butoxy]-4,4-dimethyl-4H-3,1-benzoxazin-2-one

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
40 °C

実験手順

A solution of 1.9 gm (0.01 mol) of 6-hydroxy-4,4-dimethyl-4H-3,1-benzoxazin-2-one and 4.1 gm (0.0125 mol) of 4-(3,4-dichlorophenyl-sulfinyl)-butylbromide (m.p.: 63°-64° C.) in 40 ml of dimethylsulfoxide is mixed with 3.5 gm (0.025 mol) of potassium carbonate, and the mixture is stirred for three hours at 40° C. After cooling, copious amounts of ice water are added, and the mixture is extracted with chloroform. The extract is washed with water and dried with sodium sulfate, and the chloroform is distilled off. The residue is recrystallized from isopropanol/diisopropylether.

後処理

  1. temperatureAfter cooling
  2. extractionthe mixture is extracted with chloroform
  3. washThe extract is washed with water
  4. dry with materialdried with sodium sulfate
  5. distillationthe chloroform is distilled off
  6. customThe residue is recrystallized from isopropanol/diisopropylether

出典と根拠

ORDレコード
ord-0d70346763624095a825da169f61e3c6
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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