Water → HCID 2797875、化合物

HRID 1448954ノート

反応式

HRID 1448954 の反応式
[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]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 832754-Pyridineethanamine

生成物 1

HCID 2797875HCID 2797875、化合物収率 23.7%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-8f62454c3b6c4e0e843f3c248303242a
出典データセット
uspto-grants-1980_02
特許番号
US04188391

反応ノート

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