Methanol → 4-Bromo-1-benzothiophene-2-carboxylic acid

HRID 2183608

반응식

HRID 2183608 반응식
[Br:1][C:2]1[C:10]2[CH:9]=[C:8]([C:11]([O:13]C)=[O:12])[S:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].CO>O>[Br:1][C:2]1[C:10]2[CH:9]=[C:8]([C:11]([OH:13])=[O:12])[S:7][C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 22473901Methyl 4-bromo-1-benzothiophene-2-carboxylate

생성물 1

HCID 134665384-Bromo-1-benzothiophene-2-carboxylic acid수율 64.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of methyl 4-bromobenzo[b]thiophene-2-carboxylate (101 g), sodium hydroxide (63 g), methanol (1200 ml) and water (600 ml) was stirred at ambient temperature for 16 hours, the methanol was removed in vacuo, and the resulting suspension was cooled to 0° C. and acidified by dropwise addition of concentrated hydrochloric acid. The mixture was stirred for 20 minutes and the resulting solid was collected by filtration, washed with water (3×250 ml) and dried in vacuo at 110-120° C. to give 4-bromobenzo[b]thiophene-2-carboxylic acid (62 g) as a cream solid which was used without further purification.

후처리

  1. customthe methanol was removed in vacuo
  2. temperaturethe resulting suspension was cooled to 0° C.
  3. additionacidified by dropwise addition of concentrated hydrochloric acid
  4. stirringThe mixture was stirred for 20 minutes
  5. filtrationthe resulting solid was collected by filtration
  6. washwashed with water (3×250 ml)
  7. customdried in vacuo at 110-120° C.

출처 및 근거

ORD 기록
ord-ed15c01f872b4d8d81cc4481d67bf288
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900216B2

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