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Triethylamine → HCID 67204782, 화합물

HRID 1626321
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HRID 1626321 반응식
Cl[C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[N:6]2[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.Cl.Cl.[CH3:25][C:26]1[C:31]([CH3:32])=[CH:30][CH:29]=[CH:28][C:27]=1[N:33]1[CH2:38][CH2:37][N:36]([CH2:39][CH2:40][CH2:41][NH2:42])[CH2:35][CH2:34]1.C(N(CC)CC)C>C(O)C>[CH3:25][C:26]1[C:31]([CH3:32])=[CH:30][CH:29]=[CH:28][C:27]=1[N:33]1[CH2:34][CH2:35][N:36]([CH2:39][CH2:40][CH2:41][NH:42][C:2]2[N:10]=[CH:9][N:8]=[C:7]3[C:3]=2[N:4]=[C:5]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:6]3[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:37][CH2:38]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 70664367HCID 70664367, 화합물HCID 86046565HCID 86046565, 화합물

생성물 1

HCID 67204782HCID 67204782, 화합물수율 46.1%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

To a mixture of 6-chloro-8,9-diphenyl-9H-purine (150 mg, 0.49 mmol) and 3-(4-(2,3-dimethylphenyl)piperazin-1-yl)propan-1-amine dihydrochloride (313 mg, 0.98 mmol) in ethanol (4.9 mL) was added triethyl amine (0.27 mL, 1.96 mmol) and stirred at 80° C. for 15 hrs. The resulting reaction mixture was concentrated under reduced pressure. The residue was diluted with CH2Cl2, and washed with water. The organic layer thus separated was dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The crude product thus obtained was purified by preparative HPLC (purification system, Gilson) to provide the title compound (117 mg) as a white solid.

후처리

  1. customThe resulting reaction mixture
  2. concentrationwas concentrated under reduced pressure
  3. additionThe residue was diluted with CH2Cl2
  4. washwashed with water
  5. customThe organic layer thus separated
  6. dry with materialwas dried over anhydrous MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude product thus obtained
  10. customwas purified by preparative HPLC (purification system, Gilson)

출처 및 근거

ORD 기록
ord-a7a025d91abc4fa69d2e2c0937649b25
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785453B2

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