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Water → 6-Bromo-1-(3-methoxypropyl)-3-methyl-1H-indazole

HRID 252370
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인쇄 미리보기

반응식

HRID 252370 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([Br:10])=[CH:6][C:5]=1OS(C)(=O)=O)(=O)[CH3:2].[CH3:16][O:17][CH2:18][CH2:19][CH2:20][NH:21][NH2:22].C([O-])(=O)C.[NH4+].O>CC1C=CC=CC=1C>[Br:10][C:7]1[CH:6]=[C:5]2[C:4]([C:1]([CH3:2])=[N:22][N:21]2[CH2:20][CH2:19][CH2:18][O:17][CH3:16])=[CH:9][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 517165Ammonium AcetateHCID 20516966(3-Methoxypropyl)hydrazineHCID 86071609Methanesulfonic acid 2-acetyl-5-bromophenyl ester

생성물 1

HCID 231562236-Bromo-1-(3-methoxypropyl)-3-methyl-1H-indazole

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A mixture of 10.90 g methanesulfonic acid 2-acetyl-5-bromo-phenyl ester, 7.75 g of (3-methoxy-propyl)-hydrazine and 7.17 g of ammonium acetate in 100 ml of o-xylene is refluxed for 3 days with continuous separation of the water which is formed during the reaction. The reaction mixture is then cooled to room temperature and concentrated by evaporation. The title compound is obtained as an orange-yellow oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.38 (1:1 EtOAc-heptane). Rt=4.52 (gradient I).

후처리

  1. customis formed during the reaction
  2. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-f7b92177327a47ed90865467c01f2ce8
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07868036B2

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