Hydrochloric Acid → HCID 15812073、化合物

HRID 359278ノート

反応式

HRID 359278 の反応式
O1CCCC1.[CH3:6][C:7]([NH:10][C:11]1[O:12][C:13]([C:20]([O:22]CC)=[O:21])=[C:14]([C:16]([F:19])([F:18])[F:17])[N:15]=1)([CH3:9])[CH3:8].[OH-].[Na+].Cl>O>[CH3:9][C:7]([NH:10][C:11]1[O:12][C:13]([C:20]([OH:22])=[O:21])=[C:14]([C:16]([F:17])([F:19])[F:18])[N:15]=1)([CH3:6])[CH3:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 20064741Ethyl 2-[(1,1-dimethylethyl)amino]-4-trifluoromethyl-5-oxazolecarboxylate

生成物 1

HCID 15812073HCID 15812073、化合物収率 9.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A reaction vessel was charged with 200 ml tetrahydrofuran and 28 g (100 mmol) of ethyl 2-[(1,1dimethylethyl)amino]-4-trifluoromethyl-5-oxazolecarboxylate (prepared by Example 6). With this mixture stirred at ambient temperature, 50% aqueous sodium hydroxide (16 g; 200 mmol) was added followed by 50 ml water as a rinse. The reaction mixture was stirred at ambient temperature for 16 hours. The mixture was then poured into 500 ml of 5% hydrochloric acid. After cooling with an ice bath, the mixture was filtered, washed with water, and then dried to yield 2.4 g of a white powder which was recrystallized from ethyl acetate to a crystalline product (m.p.=256°-258° C.) identified in Table I.

後処理

  1. stirringThe reaction mixture was stirred at ambient temperature for 16 hours
  2. temperatureAfter cooling with an ice bath
  3. filtrationthe mixture was filtered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-25e059f518784467abbaad415a2e5cf5
出典データセット
uspto-grants-1991_03
特許番号
US05000775

反応ノート

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