Triethylamine → HCID 15463329, 화합물

HRID 618289노트

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HRID 618289 반응식
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([O:14][C:15]([N:17]2[CH2:22][CH2:21][CH:20]([O:23][C:24](=[O:45])[NH:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][O:32][C:33](OC3C=CC([N+]([O-])=O)=CC=3)=[O:34])[CH2:19][CH2:18]2)=[O:16])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:46][C:47]([CH3:65])([CH3:64])[CH2:48][C:49]1[CH:63]=[CH:62][C:52]([CH2:53][NH:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH3:61])=[CH:51][CH:50]=1.C(N(CC)CC)C>CN(C)C=O.C(Cl)Cl>[O:1]([C:8]1[CH:9]=[CH:10][C:11]([O:14][C:15]([N:17]2[CH2:18][CH2:19][CH:20]([O:23][C:24](=[O:45])[NH:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][O:32][C:33](=[O:34])[N:54]([CH2:53][C:52]3[CH:62]=[CH:63][C:49]([CH2:48][C:47]([CH3:46])([CH3:65])[CH3:64])=[CH:50][CH:51]=3)[CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH3:61])[CH2:21][CH2:22]2)=[O:16])=[CH:12][CH:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 14995484HCID 14995484, 화합물HCID 542367634-[6-(4-Nitro-phenoxycarbonyloxy)-hexylcarbamoyloxy]-piperidine-1-carboxylic acid 4-phenoxyphenyl ester

생성물 1

HCID 15463329HCID 15463329, 화합물수율 112.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

A solution of the carbonate (2.0 g, 3.2 mmol) produced in Example 5, 4-(2,2-dimethyl-propyl)-benzyl-heptylamine (1.1 g, 3.9 mmol) and triethylamine (2.2 ml, 16 mmol) in 30 ml of anhydrous dimethylformamide was stirred under nitrogen at room temperature overnight. The reaction was diluted with methylene chloride, extracted one time with 1N HCl, multiple times with saturated Na2CO3, dried (MgSO4) and the solvent removed under reduced pressure to give 2.73 g of a light brown oil. Purification of this oil by chromatography on silica gel (230-400 mesh) using 10% ethyl acetate-methylene chloride as the eluent gave 2.11 g (87%) of the title compound as a clear oil, MS m/e 758 (M+H)+.

후처리

  1. extractionextracted one time with 1N HCl, multiple times with saturated Na2CO3
  2. dry with materialdried (MgSO4)
  3. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-140ef14d0f7f44d6b0862bf4e6fa461c
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952354

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