Ammonia → L-Asparagine, monohydrate

HRID 1728438

반응식

HRID 1728438 반응식
S(=O)(=O)(O)[OH:2].[NH2:6][C@H:7]([C:12]([OH:14])=[O:13])[CH2:8][C:9](O)=[O:10].[NH3:15]>CO>[OH2:2].[NH2:6][C@H:7]([C:12]([OH:14])=[O:13])[CH2:8][C:9](=[O:10])[NH2:15]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 5960L-Aspartic Acid

생성물 1

HCID 170358L-Asparagine, monohydrate

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
24 °C

실험 절차

A solution of 31.5 ml. sulfuric acid in 295 ml. methanol was treated with 66.5 g. L-aspartic acid, and heated at 40-45° C. for 4 hours. The solution was cooled to 24° C., and treated with 28% aqueous ammonia to a pH of 2.5. The mixture was concentrated under vacuum to a thick slurry. The slurry was treated with 750 ml. of 28% aqueous ammonia and 20 ml. water, and stirred at 24° C. for 3.5 hours. The mixture was concentrated under vacuum nearly to dryness, redissolved in 75 ml. water at 55° C., adjusted to pH of 5.4 with excess ammonia, and then cooled to 24° C. The solid was collected by filtration, washed and dried, and finally recrystallized from another 75 ml. water to yield 31.0 g asparagine monohydrate.

후처리

  1. concentrationThe mixture was concentrated under vacuum to a thick slurry
  2. additionThe slurry was treated with 750 ml
  3. concentrationThe mixture was concentrated under vacuum nearly to dryness
  4. dissolutionredissolved in 75 ml
  5. customat 55° C.
  6. temperaturecooled to 24° C
  7. filtrationThe solid was collected by filtration
  8. washwashed
  9. customdried
  10. customfinally recrystallized from another 75 ml

출처 및 근거

ORD 기록
ord-d0326cd7a0e74954b3cf17c531e61e0a
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05326908

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