Methanol → HCID 178448096, compound

HRID 1260169Notes

Reaction equation

HRID 1260169 reaction equation
[CH3:1][N:2]1[C:8](=[O:9])[N:7]([CH3:10])[C:5](=[O:6])[C:4]2[N:11]([CH2:14][CH2:15][N:16]3[CH2:21][CH2:20][N:19]([C:22]4[C:27]([Cl:28])=[CH:26][CH:25]=[CH:24][CH:23]=4)[CH2:18][CH2:17]3)[CH:12]=[N:13][C:3]1=2.[CH3:29][CH:30]([CH3:51])[C@@H:31]1[CH2:36][CH2:35][C@@H:34]([C:37]([NH:39][C@H:40]([CH2:44][C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)[C:41]([OH:43])=[O:42])=[O:38])[CH2:33][CH2:32]1.CO>C(O)C.O>[CH3:1][N:2]1[C:8](=[O:9])[N:7]([CH3:10])[C:5](=[O:6])[C:4]2[N:11]([CH2:14][CH2:15][N:16]3[CH2:21][CH2:20][N:19]([C:22]4[C:27]([Cl:28])=[CH:26][CH:25]=[CH:24][CH:23]=4)[CH2:18][CH2:17]3)[CH:12]=[N:13][C:3]1=2.[CH3:29][CH:30]([CH3:51])[C@@H:31]1[CH2:32][CH2:33][C@@H:34]([C:37]([NH:39][C@H:40]([CH2:44][C:45]2[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=2)[C:41]([OH:43])=[O:42])=[O:38])[CH2:35][CH2:36]1

Participants

6

Reactant 3

HCID 887MethanolHCID 10453764Kmup 1HCID 178448095HCID 178448095, compound

Product 1

HCID 178448096HCID 178448096, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolvent2×HCID 962WaterSolvent

Procedure

KMUP-1 (8.0 g) is dissolved in a mixture of ethanol (100 mL) and water (30 mL), to which nateglinide (9.1 g) dissolved in ethyl alcohol (150 mL) is added, and the mixture is reacted at 50° C. for 20 mins. After cooling the mixture, the white precipitate is obtained, to which the methanol is added under room temperature and being incubated over night for re-crystallization. After filtering, KMUP-1-nateglinide complex (15.3 g) is obtained.

Workup

  1. additionis added
  2. customthe mixture is reacted at 50° C. for 20 mins
  3. temperatureAfter cooling the mixture
  4. additionis added under room temperature
  5. custombeing incubated over night for re-crystallization
  6. filtrationAfter filtering
  7. customKMUP-1-nateglinide complex (15.3 g) is obtained

Sources & evidence

ORD record
ord-7f5d9e09f5554ad68d01a18d1a17ec6d
Source dataset
uspto-grants-2013_06
Patent number
US08470805B2

Reaction notes

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