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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → HCID 59758990, 화합물

HRID 914391
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인쇄 미리보기

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HRID 914391 반응식
[CH2:1]([NH:8][CH2:9][CH2:10][C:11]1[N:12]=[C:13]([S:16][C:17]([CH3:22])([CH3:21])[C:18]([OH:20])=[O:19])[S:14][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].C(N(CC)CC)C.Cl[C:31]1[C:36]([N+:37]([O-:39])=[O:38])=[CH:35][CH:34]=[CH:33][N:32]=1>C(#N)C>[CH2:1]([N:8]([C:31]1[C:36]([N+:37]([O-:39])=[O:38])=[CH:35][CH:34]=[CH:33][N:32]=1)[CH2:9][CH2:10][C:11]1[N:12]=[C:13]([S:16][C:17]([CH3:21])([CH3:22])[C:18]([OH:20])=[O:19])[S:14][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 796132-Chloro-3-nitropyridineHCID 67399150HCID 67399150, 화합물

생성물 1

HCID 59758990HCID 59758990, 화합물수율 0.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a suspension of 2-({4-[2-(heptylamino)ethyl]-1,3-thiazol-2-yl}thio)-2-methylpropionic acid resin (0.15 g) synthesized in Example 461-6 in acetonitrile (1.5 ml) were added triethylamine (0.16 ml) and 2-chloro-3-nitropyridine (0.089 g), and the mixture was stirred at room temperature overnight. The resin was collected by filtration from the mixture, washed three times with dimethylformamide, tetrahydrofuran and methanol, and vacuum dried. Trifluoroacetic acid (2.0 mL) was added to the obtained resin, and the mixture was left standing at room temperature for 2 hr. Then the resin was removed by filtration from the reaction mixture, and the filtrate was concentrated by blowing a nitrogen gas, vacuum dried, and purified by preparative HPLC to give the title compound (1.5 mg) as a pale-brown oil.

후처리

  1. filtrationThe resin was collected by filtration from the mixture
  2. washwashed three times with dimethylformamide, tetrahydrofuran and methanol, and vacuum
  3. customdried
  4. additionTrifluoroacetic acid (2.0 mL) was added to the obtained resin
  5. waitthe mixture was left
  6. waitstanding at room temperature for 2 hr
  7. customThen the resin was removed by filtration from the reaction mixture
  8. concentrationthe filtrate was concentrated
  9. customdried
  10. custompurified by preparative HPLC

출처 및 근거

ORD 기록
ord-243af8cffdef40d487b35152ecd17dc3
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08026370B2

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