Triethylamine → HCID 44159737, 화합물

HRID 1886966노트

반응식

HRID 1886966 반응식
[NH2:1][CH:2]1[C:8]2=[N:9][C:10]([C:14]3[CH:19]=[CH:18][N:17]=[CH:16][N:15]=3)=[CH:11][C:12](=[O:13])[N:7]2[CH2:6][CH2:5][O:4][CH2:3]1.[C:20]([O:24][C:25]([N:27]1[CH2:36][CH2:35][C:34]2[C:29](=[CH:30][C:31]([C:37](O)=[O:38])=[CH:32][CH:33]=2)[CH2:28]1)=[O:26])([CH3:23])([CH3:22])[CH3:21].C(P(=O)(OCC)OCC)#N.C(N(CC)CC)C>CN(C)C=O.C(OCC)(=O)C.O>[C:20]([O:24][C:25]([N:27]1[CH2:36][CH2:35][C:34]2[C:29](=[CH:30][C:31]([C:37](=[O:38])[NH:1][CH:2]3[C:8]4=[N:9][C:10]([C:14]5[CH:19]=[CH:18][N:17]=[CH:16][N:15]=5)=[CH:11][C:12](=[O:13])[N:7]4[CH2:6][CH2:5][O:4][CH2:3]3)=[CH:32][CH:33]=2)[CH2:28]1)=[O:26])([CH3:23])([CH3:21])[CH3:22]

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 189883742-((Tert-butoxy)carbonyl)-1,2,3,4-tetrahydroisoquinoline-7-carboxylic acidHCID 68626960HCID 68626960, 화합물

생성물 1

HCID 44159737HCID 44159737, 화합물수율 38.6%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 0.080 g (0.31 mmol) of (+/−)-9-Amino-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4-a-diaza-benzocyclohepten-4-one dissolved in 2.60 mL of dimethylformamide was added 0.086 g (0.31 mmol) of 3,4-dihydro-1H-isoquinoline-2,7-dicarboxylic acid 2-tert-butyl ester. To the resulting mixture was added 60 μL (0.37 mmol) of diethyl cyanophosphonate and 40 μL (0.31 mmol) of triethylamine at 0° C. The resulting mixture was stirred at room temperature for 15 hours. Water and ethyl acetate were added and the mixture was stirred. The resulting residue was filtered, washed with water, ethyl acetate and diethyl ether to afford 0.062 g (38%) of the pure product as a white powder.

후처리

  1. stirringthe mixture was stirred
  2. filtrationThe resulting residue was filtered
  3. washwashed with water, ethyl acetate and diethyl ether

출처 및 근거

ORD 기록
ord-073d483f88a04d54866a02d9abd78431
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501728B2

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