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Ammonia → 1-(7,8-Dichloro-3,4-dihydroisoquinolin-2(1H)-yl)ethan-1-one

HRID 461502
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HRID 461502 반응식
Cl.[Cl:2][C:3]1[C:12]([Cl:13])=[C:11]2[C:6]([CH2:7][CH2:8][NH:9][CH2:10]2)=[CH:5][CH:4]=1.[C:14]([O-])(=[O:16])[CH3:15].[Na+].C(OC(=O)C)(=O)C.N>O.C(O)(=O)C>[C:14]([N:9]1[CH2:8][CH2:7][C:6]2[C:11](=[C:12]([Cl:13])[C:3]([Cl:2])=[CH:4][CH:5]=2)[CH2:10]1)(=[O:16])[CH3:15]
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참가 물질

7

반응물 4

HCID 222AmmoniaHCID 7918Acetic AnhydrideHCID 1239197,8-Dichloro-1,2,3,4-tetrahydroisoquinoline hydrochlorideHCID 517045Sodium Acetate

생성물 1

HCID 125951001-(7,8-Dichloro-3,4-dihydroisoquinolin-2(1H)-yl)ethan-1-one

시약·촉매·용매 2

HCID 176Acetic Acid용매
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HCID 962
Water
용매

실험 절차

7,8-Dichloro-1,2,3,4-tetrahydroisoquinoline hydrochloride (0.001 mole) was treated with sodium acetate (0.001 mole), acetic anhydride (0.00125 mole), and 2 ml. of acetic acid and the mixture was heated at 95° C. for 15 minutes. The mixture was cooled, diluted with water, made alkaline with aqueous ammonia and extracted with chloroform. Concentration of the extract and recrystallization of the residue from isopropanol gave 2-acetyl-7,8-dichloro-1,2,3,4-tetrahydroisoquinoline, m.p. 99.5-100° C.

후처리

  1. temperatureThe mixture was cooled
  2. extractionextracted with chloroform
  3. extractionConcentration of the extract
  4. customrecrystallization of the residue from isopropanol

출처 및 근거

ORD 기록
ord-7797c1349b64444fbb7425dbf8db686c
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04062961

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