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Triethylamine → HCID 9845158、化合物

HRID 973448
ノート
印刷プレビュー

反応式

HRID 973448 の反応式
[CH2:1]([C:10]1[CH:18]=[CH:17][C:13](C(O)=O)=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].C([N:21]([CH2:24]C)CC)C.[O:26](P(N=[N+]=[N-])(OC1C=CC=CC=1)=O)C1C=CC=CC=1.[CH:45]([C:48]1[CH:54]=[CH:53][CH:52]=[C:51]([CH:55]([CH3:57])[CH3:56])[C:49]=1[NH2:50])([CH3:47])[CH3:46]>C1(C)C=CC=CC=1>[CH2:1]([C:10]1[CH:11]=[CH:12][C:13]([NH:21][C:24]([NH:50][C:49]2[C:48]([CH:45]([CH3:47])[CH3:46])=[CH:54][CH:53]=[CH:52][C:51]=2[CH:55]([CH3:57])[CH3:56])=[O:26])=[CH:17][CH:18]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 32484DiisopropylanilineHCID 380024-Nonylbenzoic acidHCID 123414Diphenylphosphoryl azide

生成物 1

HCID 9845158HCID 9845158、化合物収率 62.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a 10 ml toluene solution of 1.0 g (4.04 mmol) of 4-nonylbenzoic acid was added 0.66 ml (4.28 mmol) of triethylamine. After stirring at room temperature for 15 minutes, 0.89 ml (4.12 mmol) of DPPA (diphenoxy phosphoryl azide) was added to the mixture. The whole was heated for 2 hours under reflux and then cooled to room temperature. After the addition of 0.77 ml (4.08 mmol) of 2,6-diisopropylaniline, the reaction mixture was stirred for 16 hours and then concentrated. The residue was purified by subjecting it to column chromatography over silica gel (eluent: n-hexane/chloroform=1/1) to give 1.07 g (62% yield) of 1-(4-nonylphenyl)-3-(2,6-diisopropylphenyl)urea, the physical properties of which being shown in the following Table 3. The compounds No. 5, No. 6, No. 7, No. 8, No. 9, No. 10, No. 12, No. 16, No. 20, No. 21, No. 22, No. 23, and No. 26 listed in Table 3 were similarly prepared as above.

後処理

  1. temperatureThe whole was heated for 2 hours
  2. temperatureunder reflux
  3. temperaturecooled to room temperature
  4. stirringthe reaction mixture was stirred for 16 hours
  5. concentrationconcentrated
  6. customThe residue was purified

出典と根拠

ORDレコード
ord-31c8a23e550547048f9ab75b74705bf2
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05063247

反応ノート

読み込み中…

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