Hydrochloric Acid → HCID 14858826, 화합물

HRID 1073981

반응식

HRID 1073981 반응식
[NH2:1][C@H:2]([C:4]([N:6]1[CH2:13][CH2:12][CH2:11][C@H:7]1[C:8]([OH:10])=[O:9])=[O:5])[CH3:3].[C:14]1([CH3:26])[CH:19]=[C:18]([CH3:20])[CH:17]=[C:16]([CH3:21])[C:15]=1[S:22](Cl)(=[O:24])=[O:23].O.Cl>[OH-].[Na+].O1CCOCC1>[C:14]1([CH3:26])[CH:19]=[C:18]([CH3:20])[CH:17]=[C:16]([CH3:21])[C:15]=1[S:22]([NH:1][C@H:2]([C:4]([N:6]1[CH2:13][CH2:12][CH2:11][C@H:7]1[C:8]([OH:10])=[O:9])=[O:5])[CH3:3])(=[O:23])=[O:24]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 130462-Mesitylenesulfonyl chlorideHCID 83525L-Alanyl-L-proline

생성물 1

HCID 14858826HCID 14858826, 화합물수율 45.3%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide용매2회HCID 312751,4-Dioxane용매2회

실험 절차

L-alanyl-L-proline (1.86 g, 10 mmole) was dissolved in aqueous sodium hydroxide (10 ml)-dioxane (10 ml), and dioxane (5 ml) solution of mesitylenesulfonylchloride (2.19 g, 10 mmole) was added dropwise to the solution while cooling and stirring while keeping pH value thereof to 10 to 11 with 1N aqueous sodium hydroxide. After that; the mixture was stirred further for 2 hours at room temperature. Water (20 ml) was added thereto and the mixture thus obtained was washed with diethyl ether (40 ml). The water layer was filtered and the filtrate thus obtained was adjusted to pH 2.0 with 1N hydrochloric acid while cooling and stirring to precipitate white solid material. The material was dissolved in 0.5N aqueous sodium hydroxide and the solution thus obtained was crystallized by addition of 1N aqueous hydrochloric acid to give N-mesitylenesulfonyl-L-alanyl-L-proline yield: 1.67 g, 45.3%).

후처리

  1. additionwas added dropwise to the solution
  2. temperaturewhile cooling
  3. stirringthe mixture was stirred further for 2 hours at room temperature
  4. customthe mixture thus obtained
  5. washwas washed with diethyl ether (40 ml)
  6. filtrationThe water layer was filtered
  7. customthe filtrate thus obtained
  8. temperaturewhile cooling
  9. stirringstirring
  10. customto precipitate white solid material
  11. dissolutionThe material was dissolved in 0.5N aqueous sodium hydroxide
  12. customthe solution thus obtained
  13. customwas crystallized by addition of 1N aqueous hydrochloric acid

출처 및 근거

ORD 기록
ord-ee566e0950fc49afb6f1abac4eb7773d
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971993

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