Hydrochloric Acid → Methyl 4'-Tosylmycophenolate

HRID 260105

反応式

HRID 260105 の反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[OH:12][C:13]1[C:21]([CH2:22]/[CH:23]=[C:24](\[CH3:31])/[CH2:25][CH2:26][C:27]([O:29][CH3:30])=[O:28])=[C:20]([O:32][CH3:33])[C:19]([CH3:34])=[C:18]2[C:14]=1[C:15](=[O:35])[O:16][CH2:17]2.Cl>N1C=CC=CC=1>[CH3:33][O:32][C:20]1[C:19]([CH3:34])=[C:18]2[C:14]([C:15](=[O:35])[O:16][CH2:17]2)=[C:13]([O:12][S:7]([C:4]2[CH:5]=[CH:6][C:1]([CH3:11])=[CH:2][CH:3]=2)(=[O:9])=[O:8])[C:21]=1[CH2:22]/[CH:23]=[C:24](\[CH3:31])/[CH2:25][CH2:26][C:27]([O:29][CH3:30])=[O:28]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 73974-Toluenesulfonyl chlorideHCID 6478685Methyl (4E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate

生成物 1

HCID 10529011Methyl 4'-Tosylmycophenolate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

p-Toluenesulfonyl chloride (30 g) was added to a solution of methyl (E) 6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-4-methyl-4-hexenoate (40 g) in pyridine (200 ml) at 0° C. After 6 hours the solution was poured on to ice and acidified to pH 3 with dilute hydrochloric acid. The solution was extracted with ethyl acetate and the extract was dried and evaporated to afford methyl (E) 6-(1,3-dihydro-6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxyisobenzofuran-5-yl)-4-methyl-4-hexenoate.

後処理

  1. additionAfter 6 hours the solution was poured on to ice
  2. extractionThe solution was extracted with ethyl acetate
  3. customthe extract was dried
  4. customevaporated

出典と根拠

ORDレコード
ord-c04ce4af8d574b5f9a412bb51789186a
出典データセット
uspto-grants-1996_06
特許番号
US05525602

関連ノート

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