Water → HCID 2797875, 화합물

HRID 1164505노트

반응식

HRID 1164505 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-methanesulphonamidoethyl)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-780155ae895945a7860c0be2f63f9383
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04370328

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