Hydrochloric Acid → HCID 86604920、化合物

HRID 2283730ノート

反応式

HRID 2283730 の反応式
Cl.C([O:4][CH:5](OCC)[C:6]1[CH:7]=[C:8]([C:12]([CH3:24])([CH3:23])[CH2:13][NH:14][C:15](=[O:22])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:9]([CH3:11])[N:10]=1)C.COC(C)(C)C.C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1>[CH:5]([C:6]1[CH:7]=[C:8]([C:12]([CH3:24])([CH3:23])[CH2:13][NH:14][C:15](=[O:22])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:9]([CH3:11])[N:10]=1)=[O:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 15413tert-Butyl methyl etherHCID 66958383HCID 66958383、化合物

生成物 1

HCID 86604920HCID 86604920、化合物収率 76.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Hydrochloric acid (40 mL of 1 M) was added to a solution of N-[1-(5-diethoxymethyl-2-methyl-2H-pyrazol-3-yl)-1,1-dimethylethyl]benzamide (8.7 g, 24 mmol) in tetrahydrofuran (40 mL), and the reaction was stirred for ten minutes. tert-Butyl methyl ether and 2 M aqueous sodium carbonate (20 mL) were added. The aqueous layer was extracted twice with tert-butyl methyl ether, and the combined organic fractions were dried over magnesium sulfate and filtered. Hexane was added, and the cloudy mixture was stored overnight in the refrigerator. Crystals formed and were isolated in two crops by filtration to provide 5.24 g of N-[1-(5-formyl-2-methyl-2H-pyrazol-3-yl)-1,1-dimethylethyl]benzamide as a white powder, mp 150-151° C.

後処理

  1. extractionThe aqueous layer was extracted twice with tert-butyl methyl ether
  2. dry with materialthe combined organic fractions were dried over magnesium sulfate
  3. filtrationfiltered
  4. additionHexane was added
  5. customCrystals formed
  6. customwere isolated in two crops by filtration

出典と根拠

ORDレコード
ord-02825775aaea407d8afdea5b46d3e12d
出典データセット
uspto-grants-2015_09
特許番号
US09145410B2

反応ノート

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