Pyridinium chloride → HCID 13290001, 화합물

HRID 485854노트

반응식

HRID 485854 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]3[CH:16]=[C:15]([O:17]C)[C:14]([Cl:19])=[C:13]([Cl:20])[C:10]=3[S:11][CH:12]=2)=[CH:4][CH:3]=1.Cl.N1C=CC=CC=1>O>[Cl:19][C:14]1[C:15]([OH:17])=[CH:16][C:9]2[C:8]([C:5]3[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=3)=[CH:12][S:11][C:10]=2[C:13]=1[Cl:20]

참가 물질

4

반응물 2

HCID 10176127Pyridinium chlorideHCID 13289998HCID 13289998, 화합물

생성물 1

HCID 13290001HCID 13290001, 화합물수율 78.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 200 mg of 3-(4-chlorophenyl)-6,7-dichloro-5-methoxybenzo[b]thiophene and 1.77 g of pyridine hydrochloride is stirred and heated at 195°-205° for two and one half hours. The reaction is cooled and 20 ml of water is added. The resulting solid is collected on a filter and washed with 1N hydrochloric acid. The product is chromatographed on a silica gel-hexane column using 3:1 hexane/ether as elutent. The product is isolated and recrystallized from acetone-hexane to give 150 mg of 6,7-dichloro-3-(4-chlorophenyl)-5-hydroxybenzo[b]thiophene as a white powder, mp 174°-176°.

후처리

  1. temperatureheated at 195°-205° for two and one half hours
  2. temperatureThe reaction is cooled
  3. customThe resulting solid is collected on
  4. filtrationa filter
  5. washwashed with 1N hydrochloric acid
  6. customThe product is chromatographed on a silica gel-hexane column
  7. customThe product is isolated
  8. customrecrystallized from acetone-hexane

출처 및 근거

ORD 기록
ord-1c068af4dcb44a52bb939875df4821f1
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04537976

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