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Triethylamine → HCID 87422751、化合物

HRID 1920121
ノート
印刷プレビュー

反応式

HRID 1920121 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 8471TriethylamineHCID 10821PhenylacetyleneHCID 87422732HCID 87422732、化合物

生成物 1

HCID 87422751HCID 87422751、化合物

試薬・触媒・溶媒 3

HCID 83717Copper iodide触媒HCID 178418397HCID 178418397、化合物触媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3cc4216e2e4d406db9bd93f1a732cd24
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08168796B2

反応ノート

読み込み中…

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