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Triethylamine → HCID 87422751, 화합물

HRID 1920121
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HRID 1920121 반응식
[CH2:1]([N:3]([CH2:22][CH3:23])[C:4]1[CH:13]=[C:12]2[C:7]([C:8]([C:15]3[CH:20]=[CH:19][C:18](Br)=[CH:17][CH:16]=3)=[CH:9][C:10](=[O:14])[O:11]2)=[CH:6][CH:5]=1)[CH3:2].[C:24]1([C:30]#[CH:31])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(N(CC)CC)C>C1COCC1.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.[Cu](I)I>[CH2:1]([N:3]([CH2:22][CH3:23])[C:4]1[CH:13]=[C:12]2[C:7]([C:8]([C:15]3[CH:20]=[CH:19][C:18]([C:31]#[C:30][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:17][CH:16]=3)=[CH:9][C:10](=[O:14])[O:11]2)=[CH:6][CH:5]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 10821PhenylacetyleneHCID 87422732HCID 87422732, 화합물

생성물 1

HCID 87422751HCID 87422751, 화합물

시약·촉매·용매 3

HCID 83717Copper iodide촉매HCID 178418397HCID 178418397, 화합물촉매
HCID 8028
Tetrahydrofuran
용매

실험 절차

After charging 7.4 parts of 7-diethylamino-4-[(p-bromphenyl)]coumarin synthesized by a known method, 2.4 parts of phenylacetylene, 0.46 parts of tetrakis(triphenylphosphine)palladium(0), 0.038 parts of copper iodide and 20 ml of triethylamine in 40 ml of THF, the mixture was refluxed for 9 hours. The reaction mixture was filtered and washed with THF, and the obtained filtrate was concentrated and then diluted with water and filtered. The obtained cake was recrystallized from methanol. Upon drying under reduced pressure there was obtained 2.2 parts of 7-diethylamino-4-[4-(phenylethynyl)phenyl]coumarin having a melting point of 136-138° C.

후처리

  1. temperaturethe mixture was refluxed for 9 hours
  2. filtrationThe reaction mixture was filtered
  3. washwashed with THF
  4. concentrationthe obtained filtrate was concentrated
  5. additiondiluted with water
  6. filtrationfiltered
  7. customThe obtained cake was recrystallized from methanol
  8. customUpon drying under reduced pressure

출처 및 근거

ORD 기록
ord-3cc4216e2e4d406db9bd93f1a732cd24
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08168796B2

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