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Water → HCID 20184973, 화합물

HRID 2309315
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HRID 2309315 반응식
B(Br)(Br)Br.Cl[C:6]1[N:7]([C:15]2[CH:20]=[C:19]([O:21]C(C)C)[C:18]([Cl:25])=[CH:17][C:16]=2[Cl:26])[N:8]=[C:9]2[C:14]=1[CH2:13][CH2:12][CH2:11][CH2:10]2.O.CCOCC>ClCCl>[Cl:26][C:16]1[CH:17]=[C:18]([Cl:25])[C:19]([OH:21])=[CH:20][C:15]=1[N:7]1[CH:6]=[C:14]2[C:9]([CH2:10][CH2:11][CH2:12][CH2:13]2)=[N:8]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 25134Boron tribromideHCID 1847663-Chloro-2-(2,4-dichloro-5-propan-2-yloxyphenyl)-4,5,6,7-tetrahydroindazole

생성물 1

HCID 20184973HCID 20184973, 화합물수율 97.9%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매
2회

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온도
-78 °C

실험 절차

To a solution of 2.78 g boron tribromide in 5 ml of dichloromethane was added a solution of 3.10 g of 3-chloro-2-(2,4-dichloro-5-isopropoxyphenyl)-4,5,6,7-tetrahydro-2H-indazole VII-1 in 35 ml of dichloromethane under cooling at -78° C. in 15 minutes. The resultant mixture was stirred at -78° C. for 0.5 hours and at room temperature for 1.5 hours and mixed with water and ether at 0° C. The mixture was basified, and the aqueous layer was separated and acidified and shaken with ether. The extract was dried, concentrated and the residue was purified by silica gel chromatography, whereby 2.39 g of the titled compound II-1 was obtained.

후처리

  1. customthe aqueous layer was separated
  2. customThe extract was dried
  3. concentrationconcentrated
  4. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-5f379addacf64aeb9064cfa82d7e1475
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04695312

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