Lithium hydroxide, monohydrate → HCID 22282554, 화합물

HRID 2085341노트

반응식

HRID 2085341 반응식
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

참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 22282614HCID 22282614, 화합물

생성물 1

HCID 22282554HCID 22282554, 화합물수율 98%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a5c69832003e4cfd82995312ccb7ee3b
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06720329B2

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