Water → D-(+)-Cellobiose (CNP0226604.15)

HRID 1082331노트

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HRID 1082331 반응식
[CH2:1]([OH:23])[C@H:2]1[O:7][C@H:6]([O:8][C@H:9]2[C@H:14]([OH:15])[C@@H:13]([OH:16])[C@H:12]([OH:17])[O:11][C@@H:10]2[CH2:18][OH:19])[C@H:5]([OH:20])[C@@H:4]([OH:21])[C@@H:3]1[OH:22].[Br-].[Ca+2].[Br-].[OH2:27]>>[CH2:1]([OH:23])[C@H:2]1[O:7][C@@H:6]([O:8][C@@H:9]([C@H:14]([OH:15])[C@@H:13]([OH:16])[C:12]([OH:17])=[O:11])[C@H:10]([OH:27])[CH2:18][OH:19])[C@H:5]([OH:20])[C@@H:4]([OH:21])[C@@H:3]1[OH:22].[CH2:1]([OH:23])[C@H:2]1[O:7][C@@H:6]([O:8][C@H:9]2[C@H:14]([OH:15])[C@@H:13]([OH:16])[C@H:12]([OH:17])[O:11][C@@H:10]2[CH2:18][OH:19])[C@H:5]([OH:20])[C@@H:4]([OH:21])[C@@H:3]1[OH:22]

참가 물질

5

반응물 3

HCID 962WaterHCID 6255beta-Maltose3회HCID 5360316Calcium Bromide

생성물 2

HCID 10712D-(+)-Cellobiose (CNP0226604.15)HCID 6452827Cellobionic acid

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온도
8 °C

실험 절차

Maltose (1 kg, 2.92 moles) is dissolved into 3.8 , l deionized water with heating, in the range of about 40° C. to 60° C. , or sufficient to dissolve the maltose Calcium carbonate (381 g, 3.81 moles) and calcium bromide (51 g, 0.26 mole) are added with mixing. The solution is poured into an electrolysis chamber equipped with a cooling loop and cooled. Six volts DC are applied to opposite graphite electrodes. At 8 hour intervals, the potential is reversed. After 24 h, maltose (1 kg, 2.92 moles) is added and electrolysis is continued until essentially all of the maltose is converted to its acid form (as measured by HPLC), about 104 h total time. The solution is filtered to remove excess calcium carbonate and the pH of the filtrate is adjusted to 2.0 with sulfuric acid. The solution is cooled about 12 to 16 h to 8° C., and filtered to remove calcium sulfate. Calcium ions are removed by batch adsorption to Amberlite IRA 120 resin in the hydrogen form. The sulfate and bromide ions are removed by batch adsorption to Amberlite IRA 68 resin in the hydroxide form. The solution is spray dried with a Bowen 3 ft (1 m) flat bottom laboratory spray drier with a 2 fluid nozzle atomizer. The inlet temperature is kept at about 280° F. to 300° F. (138° C. to 149° C.) with all ports closed. The cellobionic acid is produced in the same manner from cellobiose.

후처리

  1. temperaturewith heating, in the range of about 40° C. to 60° C.
  2. additionare added
  3. additionwith mixing
  4. additionThe solution is poured into an electrolysis chamber
  5. customequipped with a cooling loop
  6. temperaturecooled
  7. waitAfter 24 h
  8. customis converted to its acid form (as measured by HPLC), about 104 h total time
  9. filtrationThe solution is filtered
  10. customto remove excess calcium carbonate
  11. filtrationfiltered
  12. customto remove calcium sulfate
  13. customCalcium ions are removed by batch adsorption to Amberlite IRA 120 resin in the hydrogen form
  14. customThe sulfate and bromide ions are removed by batch adsorption to Amberlite IRA 68 resin in the hydroxide form
  15. customdried with a Bowen 3 ft (1 m) flat bottom laboratory spray drier with a 2 fluid nozzle atomizer
  16. customis kept at about 280° F. to 300° F.
  17. custom(138° C. to 149° C.)
  18. customclosed

출처 및 근거

ORD 기록
ord-2acecd4b996343fe8a6800ac0adb0df0
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05589588

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