Citric Acid → Sufentanil Citrate

HRID 2395829

반응식

HRID 2395829 반응식
[CH3:1][CH2:2][C:3]([N:5]([C:12]1([CH2:25][O:26][CH3:27])[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C:20]2[S:24][CH:23]=[CH:22][CH:21]=2)[CH2:14][CH2:13]1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)=[O:4].Cl.[OH-].[K+].CCC(N(C1(COC)CCN(CCC2SC=CC=2)CC1)C1C=CC=CC=1)=O.[C:58]([OH:70])(=[O:69])[CH2:59][C:60]([CH2:65][C:66]([OH:68])=[O:67])([C:62]([OH:64])=[O:63])[OH:61]>O.C(O)C>[CH3:1][CH2:2][C:3]([N:5]([C:12]1([CH2:25][O:26][CH3:27])[CH2:13][CH2:14][N:15]([CH2:18][CH2:19][C:20]2[S:24][CH:23]=[CH:22][CH:21]=2)[CH2:16][CH2:17]1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)=[O:4].[CH2:65]([C:60]([OH:61])([C:62]([OH:64])=[O:63])[CH2:59][C:58]([OH:70])=[O:69])[C:66]([OH:68])=[O:67]

참가 물질

7

반응물 4

HCID 311Citric AcidHCID 14797Potassium HydroxideHCID 41693SufentanilHCID 18463211164790-60-7

생성물 1

HCID 65494Sufentanil Citrate

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Sufentanil HCl obtained in Example 8 was suspended in hot water and adjusted to pH 10-11 with 10% aqueous potassium hydroxide and extracted with ether. The organic layer washed with water, dried and evaporated to give the free base with an LC purity profile of 99.62%. An equivalent of sufentanil free base with anhydrous citric acid was warmed in 100% ethanol. After removal of ethanol the fluffy white powder was dried in the vacuum oven at 56° C. for 48 hrs. Sufentanil citrate thus obtained passed all USP tests.

후처리

  1. extractionextracted with ether
  2. washThe organic layer washed with water
  3. customdried
  4. customevaporated
  5. customto give the free base with an LC purity profile of 99.62%
  6. customAfter removal of ethanol the fluffy white powder
  7. customwas dried in the vacuum oven at 56° C. for 48 hrs

출처 및 근거

ORD 기록
ord-c4d7fd8d38be478e8f997c76ebc4fde9
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05489689

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