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Triethylamine → HCID 68857974, 화합물

HRID 491261
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HRID 491261 반응식
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5]N=1.[Cl:12][C:13]1[C:21]2[C:20]([NH:22][CH2:23][CH2:24][C:25]3[CH:30]=[CH:29][C:28]([OH:31])=[CH:27][CH:26]=3)=[N:19][CH:18]=[N:17][C:16]=2[S:15][CH:14]=1.[CH3:32]CN(CC)CC>C(Cl)Cl>[Cl:12][C:13]1[C:21]2[C:20]([NH:22][CH2:23][CH2:24][C:25]3[CH:30]=[CH:29][C:28]([O:31][C:7](=[O:8])[C:6]4[CH:5]=[CH:32][C:3]([O:2][CH3:1])=[CH:11][CH:10]=4)=[CH:27][CH:26]=3)=[N:19][CH:18]=[N:17][C:16]=2[S:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 178629506-Methoxypyridine-3-carbonyl chlorideHCID 67309598HCID 67309598, 화합물

생성물 1

HCID 68857974HCID 68857974, 화합물수율 22.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

A solution of 6-methoxynicotinoyl chloride (343 mg, 2 mmol) in CH2Cl2 (5 mL) was added dropwise to a solution of 4-{2-[(5-chlorothieno[2,3-d]pyrimidin-4-yl)amino]ethyl}phenol (611 mg, 2 mmol) and Et3N (1.0g, 10 mmol) in CH2Cl2 (5 mL) and the solution was stirred at room temperature overnight. The reaction was diluted with CH2Cl2 (20 mL) and washed with H2O, 1M NaOH, and brine. The organics were dried (Na2SO4) and filtered through silica gel. The solvent was stripped yielding 200 mg of material which was purified via HPLC giving 48mg, 0.11 mmol, 5 percent yield.

후처리

  1. washwashed with H2O, 1M NaOH, and brine
  2. dry with materialThe organics were dried (Na2SO4)
  3. filtrationfiltered through silica gel

출처 및 근거

ORD 기록
ord-3c24f56d45214d68b746b9ca54aff457
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531482B2

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