Lithium hydroxide, monohydrate → HCID 22282554、化合物

HRID 2085341ノート

反応式

HRID 2085341 の反応式
O.[OH-].[Li+].[O:4]=[S:5]1(=[O:25])[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[CH:8]([C:15]2[CH:24]=[CH:23][C:18]([C:19]([O:21]C)=[O:20])=[CH:17][CH:16]=2)[CH2:7][CH2:6]1>O.C1COCC1.CO>[O:4]=[S:5]1(=[O:25])[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[CH:8]([C:15]2[CH:24]=[CH:23][C:18]([C:19]([OH:21])=[O:20])=[CH:17][CH:16]=2)[CH2:7][CH2:6]1

参加物

6

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 22282614HCID 22282614、化合物

生成物 1

HCID 22282554HCID 22282554、化合物収率 98%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium hydroxide hydrate (0.195 g, 4.65 mmol) dissolved in water (1 mL) was added to a solution of methyl 4-(1,1-dioxido-3,4-dihydro-2H-1-benzothiopyran-4-yl)benzoate from reaction 33d (0.49 gm, 1.55 mmol) in THF (5 mL) and methanol (1 mL) under nitrogen atmosphere at room temperature. The reaction was stirred over night, concentrated then partitioned between 1 N HCl and ethyl acetate. The organic layer was washed with water, brine, dried over magnesium sulfate and concentrated to give 4-(1,1-dioxido-3,4-dihydro-2H-1-benzothiopyran-4-yl)benzoic acid (0.46 g, 98%) as an solid. MS found: (M−H)+=301.

後処理

  1. concentrationconcentrated
  2. customthen partitioned between 1 N HCl and ethyl acetate
  3. washThe organic layer was washed with water, brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-a5c69832003e4cfd82995312ccb7ee3b
出典データセット
uspto-grants-2004_04
特許番号
US06720329B2

反応ノート

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