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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dichloromethane → (2R)-2-({4-[(2,1,3-Benzothiadiazol-5-ylmethyl)amino]-1-piperidinyl}methyl)-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione hydrochloride

HRID 1943209
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HRID 1943209 반응식
[NH2:1][CH:2]1[CH2:7][CH2:6][N:5]([CH2:8][C@H:9]2[N:19]3[C:20]4[N:11]([C:12](=[O:22])[CH:13]=[CH:14][C:15]=4[N:16]=[CH:17][C:18]3=[O:21])[CH2:10]2)[CH2:4][CH2:3]1.[N:23]1[S:24][N:25]=[C:26]2[CH:31]=[C:30]([CH:32]=O)[CH:29]=[CH:28][C:27]=12.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+].[Cl:53]CCl>CO.C(Cl)(Cl)Cl>[ClH:53].[N:23]1[S:24][N:25]=[C:26]2[CH:31]=[C:30]([CH2:32][NH:1][CH:2]3[CH2:7][CH2:6][N:5]([CH2:8][C@H:9]4[N:19]5[C:20]6[N:11]([C:12](=[O:22])[CH:13]=[CH:14][C:15]=6[N:16]=[CH:17][C:18]5=[O:21])[CH2:10]4)[CH2:4][CH2:3]3)[CH:29]=[CH:28][C:27]=12
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참가 물질

8

반응물 5

HCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 27762902,1,3-Benzothiadiazole-5-carbaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 58200877(2R)-2-[(4-Amino-1-piperidinyl)methyl]-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione

생성물 1

HCID 68598539
(2R)-2-({4-[(2,1,3-Benzothiadiazol-5-ylmethyl)amino]-1-piperidinyl}methyl)-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione hydrochloride

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

(2R)-2-[(4-Amino-1-piperidinyl)methyl]-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione (50 mg, 0.166 mmol) (for a preparation see Example 16(j)) and 2,1,3-benzothiadiazole-5-carbaldehyde (25 mg, 0.918 eq.) were stirred in 9:1 v:v chloroform:methanol (1 ml) for 2.5 hours. Sodium triacetoxyborohydride (105 mg, 3.000 eq.) was then added in one portion and the mixture was stirred vigorously at room temperature for 30 min. Saturated aqueous sodium hydrogen carbonate (0.5 ml) was then added, followed by dichloromethane (10 ml) and the mixture was stirred vigorously at room temperature for 10 min and the phases were separated (hydrophobic frit). The organic phase was evaporated under reduced pressure and the crude product was purified by column chromatography on silica (eluted with 0-12% (2M NH3 in MeOH) in DCM). Appropriate fractions were combined and evaporated under reduced pressure to give the free base of the title compound as a yellow solid (41 mg).

후처리

  1. stirringthe mixture was stirred vigorously at room temperature for 30 min
  2. stirringthe mixture was stirred vigorously at room temperature for 10 min
  3. customthe phases were separated (hydrophobic frit)
  4. customThe organic phase was evaporated under reduced pressure
  5. customthe crude product was purified by column chromatography on silica (eluted with 0-12% (2M NH3 in MeOH) in DCM)
  6. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-80abed54041e471a9f8f3ea9f38c1384
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08389524B2

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