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

HRID 422580ノート

反応式

HRID 422580 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 27613913-Iodo-4-methylthiophene-2-carboxylic acid収率 100.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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)−.

後処理

  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

出典と根拠

ORDレコード
ord-2ab90379767a459f929aa5959fa81b6a
出典データセット
uspto-grants-2012_01
特許番号
US08101645B2

反応ノート

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