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Triethylamine → HCID 86759439, 화합물

HRID 1581646
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HRID 1581646 반응식
[O:1]=[C:2]1[NH:6][C:5](=[O:7])[C:4](=[CH:8][C:9]2[CH:10]=[CH:11][C:12]([O:19][CH3:20])=[C:13]([CH2:15][C:16]([OH:18])=O)[CH:14]=2)[S:3]1.[F:21][C:22]([F:31])([F:30])[C:23]1[CH:29]=[CH:28][C:26]([NH2:27])=[CH:25][CH:24]=1.C(N(CC)CC)C.P(C#N)(OCC)(OCC)=O>CN(C)C=O>[F:21][C:22]([F:30])([F:31])[C:23]1[CH:24]=[CH:25][C:26]([NH:27][C:16](=[O:18])[CH2:15][C:13]2[CH:14]=[C:9]([CH:8]=[C:4]3[S:3][C:2](=[O:1])[NH:6][C:5]3=[O:7])[CH:10]=[CH:11][C:12]=2[O:19][CH3:20])=[CH:28][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 99644-(Trifluoromethyl)anilineHCID 76257Diethyl cyanophosphonateHCID 72644366HCID 72644366, 화합물

생성물 1

HCID 86759439HCID 86759439, 화합물수율 72.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2-[5-[(2,4-Dioxothiazolidin-5-ylidene)methyl]-2-methoxyphenyl]-acetic acid (440 mg, 1.50 mmol), 4-(trifluoromethyl)aniline (242 μL, 1.50 mmol), triethylamine (210 μL, 1.51 mmol) and dehydrated N,N-dimethylformamide (5 mL) were mixed, and, under an atmosphere of argon, diethyl cyanophosphate (228 μL, 1.50 mmol) was added under cooling with ice and stirring. After stirring for 1 hour at room temperature, the mixture was allowed to stand for 3 days. The reaction mixture was poured into ice water and the precipitated crystals were collected by filtration. The crystals were washed with ethyl acetate, and then dried to obtain 472 mg (72%) of the title compound as yellow crystals.

후처리

  1. temperatureunder cooling with ice
  2. stirringAfter stirring for 1 hour at room temperature
  3. filtrationthe precipitated crystals were collected by filtration
  4. washThe crystals were washed with ethyl acetate
  5. customdried

출처 및 근거

ORD 기록
ord-b5b4a917aebf4709b0459788ad627d2a
출처 데이터셋
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06730687B1

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