Water → 2-(4-(Chlorosulfonyl)-3,5-dimethylphenoxy)acetic acid

HRID 628153ノート

反応式

HRID 628153 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:10]=[C:11]([CH3:13])[CH:12]=1)[O:5][CH2:6][C:7]([OH:9])=[O:8].[Cl:14][S:15](O)(=[O:17])=[O:16].O.C1COCC1>C(Cl)Cl>[Cl:14][S:15]([C:12]1[C:11]([CH3:13])=[CH:10][C:4]([O:5][CH2:6][C:7]([OH:9])=[O:8])=[CH:3][C:2]=1[CH3:1])(=[O:17])=[O:16]

参加物

6

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 24638Chlorosulfonic acidHCID 794053,5-Xylyloxyacetic acid

生成物 1

HCID 224793222-(4-(Chlorosulfonyl)-3,5-dimethylphenoxy)acetic acid収率 30%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

Referring to FIG. 37, to a solution of 2-(3,5-dimethylphenoxy)acetic acid (13 g, 72 mmol) in DCM (130 mL) was added dropwise a solution of ClSO3H (19.2 g, 166 mmol) in DCM (20 mL) at 0° C. The reaction mixture was stirred at 0° C. for 0.5 h. Water (100 mL) and THF (30 mL) were added and the resulting mixture was stirred for 5 min The two layers were separated and the organic layer was washed with brine (100 mL), dried over anhydrous Na2SO4 and concentrated under reduced pressure to give product as a white solid (6 g, 30% yield); 1H NMR (CDCl3, 300 MHz): δ 6.79 (s, 2H), 4.79 (s, 2H), 2.77 (s, 6H).

後処理

  1. stirringthe resulting mixture was stirred for 5 min The two layers
  2. customwere separated
  3. washthe organic layer was washed with brine (100 mL)
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-69cb46b93e624423b2c9f4b7600994cd
出典データセット
uspto-grants-2016_04
特許番号
US09309283B2

反応ノート

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