Lithium amide → HCID 13050864、化合物

HRID 371293ノート

反応式

HRID 371293 の反応式
CO[C:3]1[C:8]([O:9][CH3:10])=[CH:7][C:6]([CH3:11])=[CH:5][C:4]=1[C:12]1[O:13][CH2:14][C:15]([CH3:18])([CH3:17])[N:16]=1.[NH2-:19].[Li+]>O1CCCC1>[NH2:19][C:3]1[C:8]([O:9][CH3:10])=[CH:7][C:6]([CH3:11])=[CH:5][C:4]=1[C:12]1[O:13][CH2:14][C:15]([CH3:18])([CH3:17])[N:16]=1

参加物

4

反応物 2

HCID 24532Lithium amideHCID 130508632-(2,3-Dimethoxy-5-methylphenyl)-4,4-dimethyl-4,5-dihydro-1,3-oxazole

生成物 1

HCID 13050864HCID 13050864、化合物収率 25.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In dry tetrahydrofuran (80 ml) was dissolved 2-(2,3-dimethoxy-5-methylphenyl)-4,4-dimethyl-2-oxazoline (5 g). After addition of lithium amide (60 g), the mixture was stirred in a nitrogen gas stream at room temperature for 3 days. To the reaction mixture was added ice-water, followed by extraction with diethyl ether. The solvent layer was washed with water and dried over magnesium sulfate. The solvent was then distilled off to give a brown oil. This oil was chromatographed on silica gel to give colorless prisms (1.2 g) of 2-(2-amino-3-methoxy-5-methylphenyl)-4,4-dimethyl-2-oxazoline. m.p. 135°-137.5° C. (crystallized from diethyl ether)

後処理

  1. extractionfollowed by extraction with diethyl ether
  2. washThe solvent layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was then distilled off
  5. customto give a brown oil
  6. customThis oil was chromatographed on silica gel

出典と根拠

ORDレコード
ord-473d6072dd7c47868c896da4e1206cbb
出典データセット
uspto-grants-1985_07
特許番号
US04530845

反応ノート

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