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Triethylamine → HCID 68540408, 화합물

HRID 2243490
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HRID 2243490 반응식
[CH:1]1([CH2:7][NH2:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:9][O:10][C:11]([C:13]1[S:27][C:16]2[C:17]3[CH:18]=[CH:19][C:20]([C:24]([OH:26])=O)=[CH:21][C:22]=3[S:23][C:15]=2[C:14]=1[O:28][CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])=[O:12].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(CC)CC>CN(C=O)C.CCOC(C)=O>[CH3:9][O:10][C:11]([C:13]1[S:27][C:16]2[C:17]3[CH:18]=[CH:19][C:20]([C:24](=[O:26])[NH:8][CH2:7][CH:1]4[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]4)=[CH:21][C:22]=3[S:23][C:15]=2[C:14]=1[O:28][CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 76688CyclohexanemethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68540407HCID 68540407, 화합물

생성물 1

HCID 68540408HCID 68540408, 화합물수율 58%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

Cyclohexanemethyamine (29 μl, 0.22 mmol) was added to a mixture of 1-ethoxycarbonylmethoxy-3,8-dithia-cyclopenta[a]indene-2,6-dicarboxylic acid 2-methyl ester (42 mg, 0.11 mmol), HATU (49 mg, 0.13 mmol), and Et3N (50 1) in DMF (0.5 ml). The mixture was stirred for 2 days. Addition of EtOAc, washing with water, drying organic layers over MgSO4, filtration, and reoval of solvent in vacuo left crude material. Purification by column chromatography yielded 30 mg (58%) of 6-(cyclohexylmethylcarbamoyl)-1-ethoxycarbonylmethoxy-3,8-dithia-cyclopenta[a]indene-2-carboxylic acid methyl ester.

후처리

  1. washwashing with water
  2. customdrying organic layers
  3. filtrationover MgSO4, filtration, and reoval of solvent in vacuo
  4. waitleft crude material
  5. customPurification by column chromatography

출처 및 근거

ORD 기록
ord-8ffddf6d87ff4448afad54f54a24da9e
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07674822B2

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