2-Chloro-1,3-dimethyl-5-nitrobenzene → HCID 18614245、化合物

HRID 2268118ノート

反応式

HRID 2268118 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([OH:17])[CH:12]=[CH:13][C:14]=1[O:15][CH3:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].Cl[C:25]1[C:30]([CH3:31])=[CH:29][C:28]([N+:32]([O-:34])=[O:33])=[CH:27][C:26]=1[CH3:35]>CS(C)=O>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:12]=[CH:13][C:14]=1[O:15][CH3:16])[O:17][C:25]1[C:26]([CH3:35])=[CH:27][C:28]([N+:32]([O-:34])=[O:33])=[CH:29][C:30]=1[CH3:31])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 99205692-Chloro-1,3-dimethyl-5-nitrobenzeneHCID 135310983-(Benzyloxy)-4-methoxyphenolHCID 23665647Potassium tert-butoxide

生成物 1

HCID 18614245HCID 18614245、化合物収率 46.5%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
80 °C

実験手順

To a solution of 3-benzyloxy-4-methoxyphenol (3 g) in DMSO (2 mL) was added potassium t-butoxide (1.6 g). After 30 min, 4-chloro-3,5-dimethyl-nitrobenzene (2 g) was added and the resulting solution was heated at 80° C. for 2 h. The reaction mixture was partitioned between ethyl acetate and 1 N aqueous NaOH, and the organic layer was washed with water, brine, dried over sodium sulfate and concentrated in vacuo to afford 4-(3-benzyloxy-4-methoxyphenoxy)-3,5-dimethylnitrobenzene (1.9 g) as an orange solid.

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate and 1 N aqueous NaOH
  2. washthe organic layer was washed with water, brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-72e8b92896b64e3792988a1485bd683a
出典データセット
uspto-grants-2001_12
特許番号
US06326398B1

反応ノート

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