Methanol → HCID 66679578, 화합물

HRID 1019679노트

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HRID 1019679 반응식
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][CH2:7][C:6]([C:12]([OH:14])=[O:13])=[CH:5]2.CCN(CC)CC.[CH3:22][OH:23].CN([CH:27]=[O:28])C>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:22][O:23][C:27]([C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][CH2:7][C:6]([C:12]([OH:14])=[O:13])=[CH:5]2)=[O:28]

참가 물질

6

반응물 4

HCID 887MethanolHCID 6228DimethylformamideHCID 8471TriethylamineHCID 162276996-bromo-2H-chromene-3-carboxylic acid

생성물 1

HCID 66679578HCID 66679578, 화합물수율 66%

시약·촉매·용매 1

HCID 178418397HCID 178418397, 화합물촉매

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온도
80 °C

실험 절차

A mixture of XXXI (2 g, 7.84 mmol), Pd (PPh3)4 (1.36 g, 1.18 mmol), Et3N (3.3 mL, 23.52 mmol), MeOH (30 mL) and DMF (10 mL) was heated at 80° C. for 12 h under carbon monoxide atmosphere. After solvent removal, the residue was extracted with EtOAc and the organic phase was washed with brine, dried over Na2SO4, filtered, and evaporated. After silica gel column purification, 1.2 g of 2H-chromene-3,6-dicarboxylic acid 6-methyl ester XXXII was obtained (Yield 66%). MS: calc'd 235 (MH+), exp 235 (MH+).

후처리

  1. customAfter solvent removal
  2. extractionthe residue was extracted with EtOAc
  3. washthe organic phase was washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customAfter silica gel column purification

출처 및 근거

ORD 기록
ord-7b90075a91e442f09578b35790f4c4c3
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716285B2

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