Lithium amide → HCID 13050864, 화합물

HRID 1648944노트

반응식

HRID 1648944 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 13050864HCID 13050864, 화합물수율 25.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9a2261f7b3ce4a1cbae913f8482ca9d0
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04414226

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