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

HRID 1288478
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HRID 1288478 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
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, dilutes 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-9ed9f44bb4904e11bf51b742a59aff85
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03988339

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