Phosphorus oxide (P4O10) → 1-(6'-Methyl-2',3',4'-trimethoxybenzoyl)-2-methoxynaphthalene

HRID 611712

반응식

HRID 611712 반응식
CO[C:3]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[O:15][CH3:16])=[O:4].[CH3:17][O:18][C:19]1[CH:20]=[C:21]([CH3:29])[CH:22]=[C:23]([O:27][CH3:28])[C:24]=1[O:25][CH3:26].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>ClCCl>[CH3:29][C:21]1[C:22]([C:3]([C:5]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH:8]=[CH:7][C:6]=2[O:15][CH3:16])=[O:4])=[C:23]([O:27][CH3:28])[C:24]([O:25][CH3:26])=[C:19]([O:18][CH3:17])[CH:20]=1

참가 물질

5

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 809223,4,5-TrimethoxytolueneHCID 604022Methyl 2-methoxy-1-naphthoate

생성물 1

HCID 158708981-(6'-Methyl-2',3',4'-trimethoxybenzoyl)-2-methoxynaphthalene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 5B (2.02 g, 10 mmol), 3,4,5-trimethoxytoluene (1.82 g; 10 mmol), P2O5 (10.0 g) and dichloromethane is stirred at room temperature for 16 hours. Subsequently, the dichloromethane is distilled off and the residue is diluted with ethyl acetate. The organic phase is washed with water and concentrated. The residue is purified by column chromatography (petrol ethers:ethyl acetate, 8:2 v/v) and recrystallized from petrol ether:diisopropylether (1:1 v/v). The solid material is collected by vacuum filtration, washed with cold petrol ether:diisopropylether (1:1 v/v) and dried, yielding white crystals, 0.9 g, (24.6%) mp 72° C.

후처리

  1. distillationSubsequently, the dichloromethane is distilled off
  2. additionthe residue is diluted with ethyl acetate
  3. washThe organic phase is washed with water
  4. concentrationconcentrated
  5. customThe residue is purified by column chromatography (petrol ethers:ethyl acetate, 8:2 v/v)
  6. customrecrystallized from petrol ether:diisopropylether (1:1 v/v)
  7. filtrationThe solid material is collected by vacuum filtration
  8. washwashed with cold petrol ether:diisopropylether (1:1 v/v)
  9. customdried
  10. customyielding white crystals, 0.9 g, (24.6%) mp 72° C.

출처 및 근거

ORD 기록
ord-14eafedcae5a4def8b11fef508cb35a7
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06001883

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