Water → HCID 2797875, 화합물

HRID 1448954노트

반응식

HRID 1448954 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1.C(N(CC)CC)C.O>C(Cl)(Cl)Cl>[CH3:1][S:2]([NH:6][CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1)(=[O:4])=[O:3]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 832754-Pyridineethanamine

생성물 1

HCID 2797875HCID 2797875, 화합물수율 23.7%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Methanesulphonyl chloride (3.5 g.) was added slowly to 4-(2-aminoethyl)pyridine (3.6 g.) and triethylamine (3.0 g.) in chloroform (40 ml.). The temperature was maintained below 40° C. during the addition, after which the orange solution was left to stand at room temperature overnight. Water (50 ml.) was then added, the chloroform phase was separated, and the aqueous phase extracted with chloroform (100 ml.). The two chloroform solutions were combined, dried (MgSO4) and taken to dryness in vacuo to give a yellow oil which solidified immediately. This solid was crystallized from ethanol to yield white crystals of 4-(2-methanesulphonamido-ethyl)pyridine (1.4 g.).

후처리

  1. temperatureThe temperature was maintained below 40° C. during the addition
  2. waitafter which the orange solution was left
  3. customthe chloroform phase was separated
  4. extractionthe aqueous phase extracted with chloroform (100 ml.)
  5. dry with materialdried (MgSO4)
  6. customto give a yellow oil which
  7. customThis solid was crystallized from ethanol

출처 및 근거

ORD 기록
ord-8f62454c3b6c4e0e843f3c248303242a
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04188391

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