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Sodium hydride → 3-(1-Benzyloxy-7-chloro-isoquinolin-6-yloxy)-cyclobutylamine

HRID 402540
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HRID 402540 반응식
[H-].[Na+].[NH2:3][CH:4]1[CH2:7][CH:6]([OH:8])[CH2:5]1.[CH2:9]([O:16][C:17]1[C:26]2[C:21](=[CH:22][C:23](F)=[C:24]([Cl:27])[CH:25]=2)[CH:20]=[CH:19][N:18]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CC(N(C)C)=O>[CH2:9]([O:16][C:17]1[C:26]2[C:21](=[CH:22][C:23]([O:8][CH:6]3[CH2:7][CH:4]([NH2:3])[CH2:5]3)=[C:24]([Cl:27])[CH:25]=2)[CH:20]=[CH:19][N:18]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 457898893-AminocyclobutanolHCID 598182521-Benzyloxy-7-chloro-6-fluoro-isoquinoline

생성물 1

HCID 592248403-(1-Benzyloxy-7-chloro-isoquinolin-6-yloxy)-cyclobutylamine수율 30.5%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매3회

실험 절차

To a suspension of 459 mg (11.5 mmol) of sodium hydride (60%) in 16 mL of dimethyl acetamide was added a solution of 333 mg (3.82 mmol) of 3-amino-cyclobutanol (50) in 8 ml of dimethyl acetamide. After stirring for 60 min at room temperature a solution of 1.00 g (3.48 mmol) of 1-benzyloxy-7-chloro-6-fluoro-isoquinoline (11) in 16 ml of dimethyl acetamide was added and stirring was continued first at room temperature, then for 2 h at 50° C. until the reaction went to completion. The reaction was quenched by addition of water and the reaction mixture was extracted three times with a mixture of dichloromethane and 2-propanol (3:1). The combined organic layers were evaporated, water was added and the crude product was subjected to lyophilization to remove remainders of dimethyl acetamide. The obtained crude product was purified by silica gel chromatography to yield 377 mg of the title compound (51) as a mixture of diastereoisomers. Rt=0.85 min (Method H). Detected mass: 355.1 (M+H+).

후처리

  1. additionwas added
  2. customwas continued first at room temperature
  3. customThe reaction was quenched by addition of water
  4. extractionthe reaction mixture was extracted three times
  5. additionwith a mixture of dichloromethane and 2-propanol (3:1)
  6. customThe combined organic layers were evaporated
  7. additionwater was added
  8. customto remove remainders of dimethyl acetamide
  9. customThe obtained crude product
  10. customwas purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-cbe20d510efc4c62b7042c4f977f36cd
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08742116B2

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