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Triethylamine → HCID 11647739, 화합물

HRID 225800
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인쇄 미리보기

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HRID 225800 반응식
C(OP(C#N)(=O)OCC)C.C(N(CC)CC)C.Cl.[NH2:19][C:20]1[CH:21]=[CH:22][C:23]2[O:27][C:26]([CH3:28])=[N:25][C:24]=2[CH:29]=1.[F:30][C:31]([F:51])([F:50])[C:32]1[CH:33]=[C:34]([N:38]2[C:46]3[C:41](=[CH:42][CH:43]=[CH:44][CH:45]=3)[CH:40]=[C:39]2[C:47](O)=[O:48])[CH:35]=[CH:36][CH:37]=1>CN(C)C=O>[CH3:28][C:26]1[O:27][C:23]2[CH:22]=[CH:21][C:20]([NH:19][C:47]([C:39]3[N:38]([C:34]4[CH:35]=[CH:36][CH:37]=[C:32]([C:31]([F:51])([F:30])[F:50])[CH:33]=4)[C:46]4[C:41]([CH:40]=3)=[CH:42][CH:43]=[CH:44][CH:45]=4)=[O:48])=[CH:29][C:24]=2[N:25]=1
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참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 574403182-Methyl-1,3-benzoxazol-5-amine--hydrogen chloride (1/1)HCID 574403191-[3-(trifluoromethyl)phenyl]-1H-indole-2-carboxylic acid

생성물 1

HCID 11647739HCID 11647739, 화합물수율 46.9%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

0.091 ml (0.6 mmol) of diethylcyanophosphonate, 0.168 ml (0.6 mmol) of triethylamine and 0.111 g (0.6 mmol) of 5-amino-2-methylbenzoxazole hydrochloride are added to a solution of 0.152 g (0.5 mmol) of 1-[3-(trifluoromethyl)phenyl]-1H-indole-2-carboxylic acid (JP2001151771A2) in 3 ml of dimethylformamide. The mixture is stirred overnight at room temperature and concentrated under reduced pressure, and the residue is taken up in water and dichloromethane. After separation of the phases by settling, the organic phase is dried and evaporated under reduced pressure. The residue is purified by preparative chromatography. 0.102 g of solid is obtained.

후처리

  1. concentrationconcentrated under reduced pressure
  2. customAfter separation of the phases
  3. customthe organic phase is dried
  4. customevaporated under reduced pressure
  5. customThe residue is purified by preparative chromatography

출처 및 근거

ORD 기록
ord-116f969d737b4594a50357935f48efd6
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07557134B2

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