Aluminium lithium hydride → HCID 68554248, 화합물

HRID 2382117노트

반응식

HRID 2382117 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[F:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH2:14][N:13]([N:17]=O)[C:12]=2[CH:19]=1>C1COCC1>[F:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH2:14][N:13]([NH2:17])[C:12]=2[CH:19]=1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 866393826-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine

생성물 1

HCID 68554248HCID 68554248, 화합물수율 0.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

LiAlH4 in THF (1 M, 6.58 mL) is added to a solution of 6-fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine (0.8 g) in THF (10 mL) at 00 C. and then stirred at rt overnight. The reaction mixture is quenched with a few drops of water followed by addition of EtOAc (10 mL). The solid is filtered off and washed with EtOAc (15 mL). The filtrate is concentrated in vacuo and the residue is purified by silica gel column chromatography eluting with 15% EtOAc in heptane to afford 6-fluoro-2,3-dihydro-benzo[1,4]oxazin-4-ylamine (0.44 mg).

후처리

  1. customThe reaction mixture is quenched with a few drops of water
  2. additionfollowed by addition of EtOAc (10 mL)
  3. filtrationThe solid is filtered off
  4. washwashed with EtOAc (15 mL)
  5. concentrationThe filtrate is concentrated in vacuo
  6. customthe residue is purified by silica gel column chromatography
  7. washeluting with 15% EtOAc in heptane

출처 및 근거

ORD 기록
ord-5b9fab7643cb4a659da22f22c61899dd
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258130B2

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