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Hydrochloric Acid → 4-[5-(3-Dimethylaminomethyl-phenyl)-2H-[1,2,4]triazol-3-yl]-phenol hydrochloride salt

HRID 1386925
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HRID 1386925 반응식
[ClH:1].C[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[NH:14][N:13]=[C:12]([C:15]3[CH:16]=[C:17]([CH:22]=[CH:23][CH:24]=3)[CH2:18][N:19]([CH3:21])[CH3:20])[N:11]=2)=[CH:6][CH:5]=1.B(Br)(Br)Br.C([O-])([O-])=O.[Na+].[Na+].Cl>C(Cl)Cl.CO>[ClH:1].[CH3:21][N:19]([CH2:18][C:17]1[CH:16]=[C:15]([C:12]2[N:11]=[C:10]([C:7]3[CH:6]=[CH:5][C:4]([OH:3])=[CH:9][CH:8]=3)[NH:14][N:13]=2)[CH:24]=[CH:23][CH:22]=1)[CH3:20]
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 25134Boron tribromideHCID 21180376{3-[5-(4-methoxy-phenyl)-1H-[1,2,4]triazol-3-yl]-benzyl}-dimethylamine hydrochloride

생성물 1

HCID 1357941164-[5-(3-Dimethylaminomethyl-phenyl)-2H-[1,2,4]triazol-3-yl]-phenol hydrochloride salt수율 73%

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 6344Dichloromethane용매

실험 절차

A solution of {3-[5-(4-methoxy-phenyl)-1H-[1,2,4]triazol-3-yl]-benzyl}-dimethylamine hydrochloride (1:1) (100 mg, 0.29 mmol) in CH2Cl2 (5 ml) at −78° C. was treated with boron tribromide (1M CH2Cl2 1.5 ml, 1.5 mmol, 5.2 eq.). Over 16 hrs. the temperature was raised gradually to r.t. After addition of methanol (1 ml) and saturated Na2CO3 (10 ml) the pH was adjusted to 9 with 2N HCl. After extraction with CH2Cl2, then EtOAc, the combined extracts were dried with Na2SO4 and the solvent evaporated. The residue was dissolved in EtOH, 1.45M HCl/EtOH added (0.17 ml, 1.1 eq.) and stirred for 30 min. then evaporated to dryness and the product obtained was dried under high vacuum at 20° C., affording the title compound (70 mg, 73% yield) as a light yellow solid. MS: m/e=295.3 (M+H+).

후처리

  1. extractionAfter extraction with CH2Cl2
  2. dry with materialEtOAc, the combined extracts were dried with Na2SO4
  3. customthe solvent evaporated
  4. dissolutionThe residue was dissolved in EtOH
  5. addition1.45M HCl/EtOH added (0.17 ml, 1.1 eq.)
  6. customthen evaporated to dryness
  7. customthe product obtained
  8. customwas dried under high vacuum at 20° C.

출처 및 근거

ORD 기록
ord-87fa38c32a1b4ab399113e4766c7af16
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06265426B1

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