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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → [4-(5-Chloro-isoquinolin-6-yloxy)-cyclohexyl]-cyclohexyl-amine

HRID 2370737
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HRID 2370737 반응식
[Cl:1][C:2]1[C:11]([O:12][CH:13]2[CH2:18][CH2:17][C:16](=O)[CH2:15][CH2:14]2)=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][N:6]=[CH:7]2.C(N(CC)CC)C.[CH:27]1([NH2:33])[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1.C(O)(=O)C.C([BH3-])#N.[Na+]>CO>[Cl:1][C:2]1[C:11]([O:12][CH:13]2[CH2:18][CH2:17][CH:16]([NH:33][CH:27]3[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]3)[CH2:15][CH2:14]2)=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][N:6]=[CH:7]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 7965CyclohexylamineHCID 8471TriethylamineHCID 5003444Sodium cyanoborohydrideHCID 592685134-(5-Chloro-isoquinolin-6-yloxy)-cyclohexanone

생성물 1

HCID 25055878[4-(5-Chloro-isoquinolin-6-yloxy)-cyclohexyl]-cyclohexyl-amine수율 53.4%

시약·촉매·용매

1
HCID 887Methanol용매2회

실험 절차

100 mg (0.36 mmol) 4-(5-Chloro-isoquinolin-6-yloxy)-cyclohexanone (79) were dissolved in 10 ml methanol. After adding 73 mg (0.73 mmol) triethyl amine, 108 mg (1.09 mmol) cyclohexylamine, 218 mg (3.63 mmol) acetic acid and freshly dried molecular sieves, the reaction was stirred at room temperature. After 30 minutes, a solution of 68 mg (1.09 mmol) sodium cyanoborohydride in 2 ml methanol was added and the reaction was kept at room temperature until complete conversion was achieved. For working up, the reaction mixture was filtered and the filtrate was brought to alkaline pH by adding solid NaHCO3. After evaporation of the solvent, the residue was taken up in H2O and extracted three times with dichloromethane. The combined organic layers were dried over MgSO4 and evaporated. Final purification by preparative HPLC gave 69 mg of the desired product as trifluoroacetate, which was dissolved in 2 N HCl and lyophilized, to yield 45 mg of the corresponding HCl-salt. Rt=1.08/1.15 min (Method #1). Detected mass: 359.3/361.3 (M+H+).

후처리

  1. customwas kept at room temperature until complete conversion
  2. filtrationthe reaction mixture was filtered
  3. additionby adding solid NaHCO3
  4. customAfter evaporation of the solvent
  5. extractionextracted three times with dichloromethane
  6. dry with materialThe combined organic layers were dried over MgSO4
  7. customevaporated
  8. customFinal purification by preparative HPLC

출처 및 근거

ORD 기록
ord-de6808444b6545f08031604e66d1b1d7
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08710228B2

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