Hydrochloric Acid → 2-Phenoxymethyl-5-methylbenzoic Acid

HRID 894188

反応式

HRID 894188 の反応式
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][O:7][C:8]2=[O:9])=[CH:4][CH:3]=1.[C:12]1([O-:18])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Na+].Cl>O>[O:18]([CH2:6][C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:11][C:10]=1[C:8]([OH:7])=[O:9])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6387566-MethylphthalideHCID 4445035Phenolate Sodium

生成物 1

HCID 211627312-Phenoxymethyl-5-methylbenzoic Acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Stir a mixture of 1.0 gm of 6-methylphthalide and 0.64 gm of sodium phenolate at a temperature of 200°-210° C. for 1 hour. Cool and dissolve the reaction mixture in water. Acidify with 5% hydrochloric acid and extract with ether. Evaporate to dryness and chromatograph the residue over silica gel eluting with chloroform/methanol (50:1). Evaporate the eluate to dryness and crystallize the residue from ethyl acetate/benzene to obtain the title product.

後処理

  1. temperatureCool
  2. extractionextract with ether
  3. customEvaporate to dryness and chromatograph the residue over silica gel eluting with chloroform/methanol (50:1)
  4. customEvaporate the eluate to dryness
  5. customcrystallize the residue from ethyl acetate/benzene

出典と根拠

ORDレコード
ord-b246f9bd4a88459493a5078507417c1d
出典データセット
uspto-grants-1981_08
特許番号
US04282365

関連ノート

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