Methanol → HCID 178419105、化合物

HRID 345011

反応式

HRID 345011 の反応式
[NH2:1][C@H:2]([C:9]([OH:11])=[O:10])[CH2:3][C:4]1[N:8]=[CH:7][NH:6][CH:5]=1.S(Cl)([Cl:14])=O.[CH3:16]O>>[ClH:14].[ClH:14].[NH2:1][C@H:2]([C:9]([O:11][CH3:16])=[O:10])[CH2:3][C:4]1[N:8]=[CH:7][NH:6][CH:5]=1

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 178419078HCID 178419078、化合物

生成物 1

HCID 178419105HCID 178419105、化合物

実験手順

To a stirred solution (ice-bath) of L-histidine (38.75 g, 240 mmol) in methanol (500 ml), thionyl chloride (27.2 ml, 375 mmol) was added in drops. After fifteen minutes the ice bath was removed and the reaction mixture was stirred at room temperature for one hour. Then after refluxing for 48 hours, it was concentrated in vacuo. The separated crystals were filtered using methanol for washing (48.93 g). The methanolic solution on dilution with ether afforded additional 10 g of the title I compound, m.p. 208-209°.

後処理

  1. customAfter fifteen minutes the ice bath was removed
  2. temperatureThen after refluxing for 48 hours
  3. concentrationit was concentrated in vacuo
  4. filtrationThe separated crystals were filtered
  5. washfor washing (48.93 g)

出典と根拠

ORDレコード
ord-4651dec55504439d97417bbdfd2b0ee9
出典データセット
uspto-grants-1991_10
特許番号
US05055466

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