Boron trifluoride etherate → 6,7-Dichloro-5-methoxybenzo[b]thiophene

HRID 1903438노트

반응식

HRID 1903438 반응식
[Cl:1][C:2]1[C:3]([O:13][CH3:14])=[CH:4][C:5]2[CH:9](O)[CH2:8][S:7][C:6]=2[C:11]=1[Cl:12].B(F)(F)F.CCOCC.[OH-].[Na+]>C(O)(=O)C>[Cl:1][C:2]1[C:3]([O:13][CH3:14])=[CH:4][C:5]2[CH:9]=[CH:8][S:7][C:6]=2[C:11]=1[Cl:12]

참가 물질

5

반응물 3

HCID 8000Boron trifluoride etherateHCID 14798Sodium HydroxideHCID 132902146,7-Dichloro-2,3-dihydro-3-hydroxy-5-methoxybenzo[b]thiophene

생성물 1

HCID 132899966,7-Dichloro-5-methoxybenzo[b]thiophene수율 100%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 0.7 g of 6,7-dichloro-2,3-dihydro-3-hydroxy-5-methoxybenzo[b]thiophene, 1 ml of boron trifluoride etherate and 4 ml of glacial acetic acid is heated at 100° for 5 min. Ice is added and the mixture is basified with dilute sodium hydroxide solution. The off-white solid is collected on a filter, air-dried and recrystallized from ether-hexane to give 0.65 g of 6,7-dichloro-5-methoxybenzo[b]thiophene as prisms, mp 103°-104.5°.

후처리

  1. temperatureis heated at 100° for 5 min
  2. additionIce is added
  3. customThe off-white solid is collected on a filter
  4. customair-dried
  5. customrecrystallized from ether-hexane

출처 및 근거

ORD 기록
ord-4e8185be29c54d2499b66038f6e3070c
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04436748

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