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Triethylamine → HCID 86759439、化合物

HRID 1581646
ノート
印刷プレビュー

反応式

HRID 1581646 の反応式
[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
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 99644-(Trifluoromethyl)anilineHCID 76257Diethyl cyanophosphonateHCID 72644366HCID 72644366、化合物

生成物 1

HCID 86759439HCID 86759439、化合物収率 72.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b5b4a917aebf4709b0459788ad627d2a
出典データセット
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06730687B1

反応ノート

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