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Triethylamine → HCID 9845158, 화합물

HRID 973448
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HRID 973448 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 9845158HCID 9845158, 화합물수율 62.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-31c8a23e550547048f9ab75b74705bf2
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05063247

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