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Hydrochloric Acid → 6-Methoxy-1-methyl-1,2,3,4-tetrahydroisoquinoline

HRID 275896
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HRID 275896 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([CH3:13])=[N:8][CH2:7][CH2:6]2.[BH4-].[Na+].Cl.[OH-].[Na+]>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]([CH3:13])[NH:8][CH2:7][CH2:6]2
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 138591866-Methoxy-1-methyl-3,4-dihydroisoquinoline

생성물 1

HCID 142302816-Methoxy-1-methyl-1,2,3,4-tetrahydroisoquinoline수율 82,627.602%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

6-methoxy-1-methyl-3,4-dihydroisoquinoline (54.0 g, 0.31 mmol) was added to a suspension of sodium borohydride(5.8 g, 138 mmol) in ethanol. The mixture solution was stirred for 1 hour at a room temperature, cooled to below 5° C., acidified with diluted hydrochloric acid, adjusted to alkali with sodium hydroxide solution, and then extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous sodium sulfate and concentrated under a reduced pressure to give 45.4 g of the titled compound.

후처리

  1. temperaturecooled to below 5° C.
  2. extractionextracted with ethyl acetate
  3. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-0d7c703eacdf49228d4185d8be026748
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06352993B1

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