Hydrochloric Acid → 3'-Chloro-4-(1,5-dimethyl-1h-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2h-[1,2']bipyrazinyl hydrochloride salt

HRID 220546

반응식

HRID 220546 반응식
CO.C([Cl:6])(=O)C.[Cl:7][C:8]1[C:9]([N:14]2[CH2:19][CH2:18][N:17]([CH2:20][C:21]3[CH:22]=[N:23][N:24]([CH3:27])[C:25]=3[CH3:26])[CH2:16][CH2:15]2)=[N:10][CH:11]=[CH:12][N:13]=1.Cl>C1(C)C=CC=CC=1>[ClH:6].[Cl:7][C:8]1[C:9]([N:14]2[CH2:15][CH2:16][N:17]([CH2:20][C:21]3[CH:22]=[N:23][N:24]([CH3:27])[C:25]=3[CH3:26])[CH2:18][CH2:19]2)=[N:10][CH:11]=[CH:12][N:13]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 6367Acetyl chlorideHCID 594382163'-chloro-4-(1,5-dimethyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl

생성물 1

HCID 866416613'-Chloro-4-(1,5-dimethyl-1h-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2h-[1,2']bipyrazinyl hydrochloride salt수율 87%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
2 °C

실험 절차

Charge a 2 L 3-neck round bottom flask with methanol (95 mL) and chill to 2° C. and slowly add acetyl chloride (7.62 mL, 0.107 mol) dropwise under nitrogen. In a separate 1 L 3-neck flask, dissolve 3′-chloro-4-(1,5-dimethyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (36.5 g, 0.107 mol) in toluene (365 mL). Add this solution to the methanolic HCl solution in one portion. Stir vigorously for 1 hr. and concentrate to one half volume and filter to give 3′-chloro-4-(1,5-dimethyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl hydrochloride as a white solid (25.5 g, 87%). MS (ES): m/z=307.0 [M+H]+.

후처리

  1. concentrationand concentrate to one half volume
  2. filtrationfilter

출처 및 근거

ORD 기록
ord-9413431bc6a8486aa42bb4b038323059
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202873B2

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