Hydrochloric Acid → (E)-2-[3-(4-acetoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-prop-1-en-1-yl]-3-methylbenzoic acid

HRID 2396650ノート

反応式

HRID 2396650 の反応式
[C:1]([O:4][C:5]1[C:13]([CH2:14]/[CH:15]=[CH:16]/[C:17]2[C:26]([CH3:27])=[CH:25][CH:24]=[CH:23][C:18]=2[C:19]([O:21]C)=[O:20])=[C:12]([O:28][CH3:29])[C:11]([CH3:30])=[C:10]2[C:6]=1[C:7](=[O:31])[O:8][CH2:9]2)(=[O:3])[CH3:2].[OH-].[Li+].Cl>CO.O>[C:1]([O:4][C:5]1[C:13]([CH2:14]/[CH:15]=[CH:16]/[C:17]2[C:26]([CH3:27])=[CH:25][CH:24]=[CH:23][C:18]=2[C:19]([OH:21])=[O:20])=[C:12]([O:28][CH3:29])[C:11]([CH3:30])=[C:10]2[C:6]=1[C:7](=[O:31])[O:8][CH2:9]2)(=[O:3])[CH3:2]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 86749277methyl (E) 2-[3-(4-acetoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-prop-1-en-1-yl]-3-methylbenzoate

生成物 1

HCID 19046326(E)-2-[3-(4-acetoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-prop-1-en-1-yl]-3-methylbenzoic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

A solution of methyl (E)-2-[3-(4-acetoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-prop-1-en-1-yl]-3-methylbenzoate (0.1 g) and lithium hydroxide (0.06 g) in methanol (1 ml) and water (1 ml) was heated at 70° C. for 48 hours. The solution was cooled and poured into water, then acidified with 2N hydrochloric acid and extracted with ethyl acetate. The extract was dried and evaporated to give (E)-2-[3-(4-acetoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-prop-1-en-1-yl]-3-methylbenzoic acid, mp 180°-3° C. (ethyl acetate/cyclohexane).

後処理

  1. temperatureThe solution was cooled
  2. extractionextracted with ethyl acetate
  3. customThe extract was dried
  4. customevaporated

出典と根拠

ORDレコード
ord-db357d8bb11f4485a2ebb5572d1e5f09
出典データセット
uspto-grants-1996_02
特許番号
US05493030

反応ノート

読み込み中…