Propane sultone → 1,2,3,4-Tetrahydroquinoline-N-propanesulphonic acid

HRID 231034

반응식

HRID 231034 반응식
[CH2:1]1[S:5](=[O:7])(=[O:6])[O:4][CH2:3][CH2:2]1.[NH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][CH2:9]1>CO>[N:8]1([CH2:3][CH2:2][CH2:1][S:5]([OH:4])(=[O:7])=[O:6])[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][CH2:9]1

참가 물질

4

반응물 2

HCID 14264Propane sultoneHCID 694601,2,3,4-Tetrahydroquinoline

생성물 1

HCID 92497391,2,3,4-Tetrahydroquinoline-N-propanesulphonic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

48.8 molten propane-1,3-sultone were added dropwise at 60+ to 80° C. within the course of 50 minutes to 58.4 g 1,2,3,4-tetrahydroquinoline in a 500 ml. flask. The reaction mixture was left for 3.45 hours at about 70° C. and subsequently 470 ml. methanol were added portionwise under reflux conditions and further stirred under reflux conditions until the solid, glasslike under material had dissolved completely. Thereafter, the reaction mixture was cooled to ambient temperature, while stirring, a rapid crystallization thereby taking place. After leaving to stand for about 12 hours in a refrigerator, the crystals were filtered off. Yield about 50 g.; m.p. 233°-237° C.

후처리

  1. dissolutionhad dissolved completely
  2. stirringwhile stirring
  3. customa rapid crystallization
  4. customAfter leaving
  5. waitto stand for about 12 hours in a refrigerator
  6. filtrationthe crystals were filtered off

출처 및 근거

ORD 기록
ord-a5d6c7e92cdf434286cb8502d02db8d3
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845030

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