Methanol → 476199-03-8

HRID 2220307ノート

反応式

HRID 2220307 の反応式
[F:1][C:2]1[C:10]2[S:9][C:8]([C:11]([O:13]C)=[O:12])=[CH:7][C:6]=2[C:5]([O:15][CH3:16])=[CH:4][CH:3]=1.[OH-].[Na+].CO>O>[F:1][C:2]1[C:10]2[S:9][C:8]([C:11]([OH:13])=[O:12])=[CH:7][C:6]=2[C:5]([O:15][CH3:16])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 22171205Methyl 7-fluoro-4-methoxy-1-benzothiophene-2-carboxylate

生成物 1

HCID 23568964476199-03-8収率 97%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

A mixture of methyl 7-fluoro-4-methoxy-1-benzothiophene-2-carboxylate (67.2 g, 280 mmol), sodium hydroxide (45 g, 1.12 mol), methanol (800 mL) and water (400 mL) were stirred at ambient overnight. The methanol was evaporated and the mixture cooled to 0° C. Acidified with concentrated hydrochloric acid and stirred for 20 mins. The yellow solid was filtered, washing with water (3×100 mL). Dried under vacuum at 45° C. overnight, over phosphorus pentoxide to give the title compound (61.4 g, 97%); δH (300 MHz, d6-DMSO) 8.10 (1H, d, ArH) 7.44 (1H, t, ArH) 7.00 (1H, m, ArH) and 4.02 (3H, s, OCH3).

後処理

  1. customThe methanol was evaporated
  2. stirringAcidified with concentrated hydrochloric acid and stirred for 20 mins
  3. filtrationThe yellow solid was filtered
  4. washwashing with water (3×100 mL)
  5. dry with materialDried under vacuum at 45° C. overnight, over phosphorus pentoxide

出典と根拠

ORDレコード
ord-641be7131acf4ab9b2456b4687512741
出典データセット
uspto-grants-2008_08
特許番号
US07417064B2

反応ノート

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