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

HRID 231034

反応式

HRID 231034 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a5d6c7e92cdf434286cb8502d02db8d3
出典データセット
uspto-grants-1989_07
特許番号
US04845030

関連ノート

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