Hydrochloric Acid → 3-Iodo-4-methylthiophene-2-carboxylic acid

HRID 422580노트

반응식

HRID 422580 반응식
[I:1][C:2]1[C:6]([CH3:7])=[CH:5][S:4][C:3]=1[C:8]([O:10]C)=[O:9].[OH-].[Na+].CO.Cl>C1COCC1>[I:1][C:2]1[C:6]([CH3:7])=[CH:5][S:4][C:3]=1[C:8]([OH:10])=[O:9]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 2761204Methyl 3-iodo-4-methylthiophene-2-carboxylate

생성물 1

HCID 27613913-Iodo-4-methylthiophene-2-carboxylic acid수율 100.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 3-iodo-4-methylthiophene-2-carboxylate [Oakwood Product Inc.] (10 g, 35.4 mmol) in THF (200 mL) was added a solution of 2N NaOH (19.50 mL, 39.0 mmol). MeOH was added to the reaction mixture until a homogeneous solution was obtained. After about 4 h, concentrated HCl was added until a pH of about 1 was obtained. The reaction mixture was partially concentrated under reduced pressure and the resulting solid was collected by filtration and dried under reduced pressure to provide the title compound as a brown solid (9.50 g, 100%): LC/MS (Table 1, Method a) Rt=2.55 min; m/z: 267 (M−H)−.

후처리

  1. customwas obtained
  2. customwas obtained
  3. concentrationThe reaction mixture was partially concentrated under reduced pressure
  4. filtrationthe resulting solid was collected by filtration
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-2ab90379767a459f929aa5959fa81b6a
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101645B2

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