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Methyl chloroformate → 4,5-Bis(methoxycarbonyloxy)-9,10-dihydro-9,10-dioxo-2-anthracenecarboxylic acid butyl ester

HRID 2379454
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HRID 2379454 반응식
[CH2:1]([O:5][C:6]([C:8]1[CH:21]=[C:20]([OH:22])[C:19]2[C:18](=[O:23])[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][C:16]=3[OH:24])[C:11](=[O:25])[C:10]=2[CH:9]=1)=[O:7])[CH2:2][CH2:3][CH3:4].C(N(CC)CC)C.Cl[C:34]([O:36][CH3:37])=[O:35]>O1CCCC1>[CH2:1]([O:5][C:6]([C:8]1[CH:21]=[C:20]([O:22][C:34]([O:36][CH3:37])=[O:35])[C:19]2[C:18](=[O:23])[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][C:16]=3[O:24][C:6]([O:5][CH3:1])=[O:7])[C:11](=[O:25])[C:10]=2[CH:9]=1)=[O:7])[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 54443434HCID 54443434, 화합물

생성물 1

HCID 539595674,5-Bis(methoxycarbonyloxy)-9,10-dihydro-9,10-dioxo-2-anthracenecarboxylic acid butyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2.7 g (8 mmoles) of the product of Example 15 are dissolved in 100 ml of anhydrous tetrahydrofuran; the resulting solution is added first with 2.42 g (24 mmoles) of anhydrous triethylamine, then, after cooling to 0°-5° C., with 1.6 g (17 mmoles) of methyl chloroformate. The reaction is complete within 3 hours, keeping room temperature. After that, solvent is evaporated off under reduced pressure and the residue is washed with acidulated water, the product is filtered, washed and crystallized from ethyl ether. M.p. 200°-202° C.

후처리

  1. customkeeping room temperature
  2. customAfter that, solvent is evaporated off under reduced pressure
  3. washthe residue is washed with acidulated water
  4. filtrationthe product is filtered
  5. washwashed
  6. customcrystallized from ethyl ether

출처 및 근거

ORD 기록
ord-6d69df4340aa4cb18c0a07cb697980be
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05362750

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