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

反応式

HRID 220546 の反応式
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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
2 °C

実験手順

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]+.

後処理

  1. concentrationand concentrate to one half volume
  2. filtrationfilter

出典と根拠

ORDレコード
ord-9413431bc6a8486aa42bb4b038323059
出典データセット
uspto-grants-2012_06
特許番号
US08202873B2

関連ノート

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