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Methanol → 8-Carboxy-2-(dipropylamino)tetralin

HRID 1682579
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반응식

HRID 1682579 반응식
Cl.[CH2:2]([N:5]([CH2:20][CH2:21][CH3:22])[CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[C:9]([C:16]([O:18]C)=[O:17])[CH:10]=[CH:11][CH:12]=2)[CH2:7]1)[CH2:3][CH3:4].[OH-].[Na+].CO>O>[C:16]([C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:8]=1[CH2:7][CH:6]([N:5]([CH2:20][CH2:21][CH3:22])[CH2:2][CH2:3][CH3:4])[CH2:15][CH2:14]2)([OH:18])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 19044854Methyl 2-(dipropylamino)tetralin-8-carboxylate hydrochloride

생성물 1

HCID 103786878-Carboxy-2-(dipropylamino)tetralin수율 97.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of methyl 2-(dipropylamino)tetralin-8-carboxylate hydrochloride (1.5 g, 4.6 mmol), sodium hydroxide (736 mg, 18.4 mmol), methanol (25 ml) and water (4 ml) was stirred overnight, The methanol was evaporated. Concentrated hydrochloric acid was added until the pH became about 6. The solution was extracted with chloroform. The organic layer was dried (sodium sulfate) and concentrated to give 1.23 g (97%) of pure 8-carboxy-2-(dipropylamino)tetralin as an oil. The hydrochloride melts at 245°-247° C., which could bse recrystallised from methanol/diethylether.

후처리

  1. customThe methanol was evaporated
  2. additionConcentrated hydrochloric acid was added until the pH
  3. extractionThe solution was extracted with chloroform
  4. dry with materialThe organic layer was dried (sodium sulfate)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8495940f383342b5b7953186a1f6d85c
출처 데이터셋
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05635537

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