Sucralose 6-acetate → (2R,3S,4R,5R,6S)-2-[(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxyoxolan-2-yl]oxy-5-chloro-6-(hydroxymethyl)oxane-3,4-diol

HRID 1865157

반응식

HRID 1865157 반응식
CC([O:4][CH2:5][C@H:6]1[O:11][C@H:10]([O:12][C@:13]2([CH2:22][Cl:23])[O:17][C@H:16]([CH2:18][Cl:19])[C@@H:15]([OH:20])[C@@H:14]2[OH:21])[C@H:9]([OH:24])[C@@H:8]([OH:25])[C@H:7]1[Cl:26])=O.C[O-].[Na+]>CO>[CH2:5]([OH:4])[C@@H:6]1[O:11][C@H:10]([O:12][C@:13]2([CH2:22][Cl:23])[O:17][C@H:16]([CH2:18][Cl:19])[C@@H:15]([OH:20])[C@@H:14]2[OH:21])[C@@H:9]([OH:24])[C@@H:8]([OH:25])[C@H:7]1[Cl:26]

참가 물질

4

실험 절차

A mixture of 20 g of dry sucralose-6-acetate obtained from Example 5 and 70 ml of methanol was heated to from 40° C. to 50° C. When the reacting mixture became a clear solution, a small quantity of a 30% sodium methylate solution was added. After the mixture was stirred for 2 hours, methanol was removed under reduced pressure. The resultant mixture was diluted to a 30% mixture by adding a certain quantity of water, which was decolored and then filtered. The filtrate thus obtained was concentrated to a 65% solution, which was cooled to form crystallized sucralose. The obtained crystal was filtered and dried to give sucralose with a yield of over 95% and purity of over 98.0%.

후처리

  1. temperaturewas heated to from 40° C. to 50° C
  2. custommethanol was removed under reduced pressure
  3. additionThe resultant mixture was diluted to a 30% mixture
  4. additionby adding a certain quantity of water, which
  5. filtrationfiltered
  6. customThe filtrate thus obtained
  7. concentrationwas concentrated to a 65% solution, which
  8. temperaturewas cooled
  9. customto form
  10. customcrystallized sucralose
  11. filtrationThe obtained crystal was filtered
  12. customdried

출처 및 근거

ORD 기록
ord-89542098a95b4599bac600c077c6b4da
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07626016B2

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