Methanol → HCID 178419105, 화합물

HRID 345011

반응식

HRID 345011 반응식
[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

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 178419078HCID 178419078, 화합물

생성물 1

HCID 178419105HCID 178419105, 화합물

실험 절차

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°.

후처리

  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)

출처 및 근거

ORD 기록
ord-4651dec55504439d97417bbdfd2b0ee9
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055466

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