Formic Acid → Candesartan Cilexetil

HRID 11804

반응식

HRID 11804 반응식
[CH3:1][CH2:2][O:3][C:4]1[N:12]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[C:25]([C:26]4[N:30](C(C5C=CC=CC=5)(C5C=CC=CC=5)C5C=CC=CC=5)[N:29]=[N:28][N:27]=4)=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:16][CH:15]=2)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[C:50]([O:52][CH:53]([O:55][C:56]([O:58][CH:59]2[CH2:64][CH2:63][CH2:62][CH2:61][CH2:60]2)=[O:57])[CH3:54])=[O:51])[N:5]=1.C1(C)C=CC=CC=1.C(O)=O>CO>[CH3:1][CH2:2][O:3][C:4]1[N:12]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:25]=3[C:26]3[N:27]=[N:28][NH:29][N:30]=3)=[CH:16][CH:15]=2)[C:11]2[C:10]([C:50]([O:52][CH:53]([O:55][C:56]([O:58][CH:59]3[CH2:60][CH2:61][CH2:62][CH2:63][CH2:64]3)=[O:57])[CH3:54])=[O:51])=[CH:9][CH:8]=[CH:7][C:6]=2[N:5]=1

참가 물질

5

반응물 3

HCID 284Formic AcidHCID 1140TolueneHCID 11029254Trityl candesartan cilexetil

생성물 1

HCID 2540Candesartan Cilexetil

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Typically, the deprotection step comprises heating to reflux trityl candesartan cilexetil in methanol. Optionally, the deprotection solvent mixture further comprises an organic solvent, such as toluene, and/or an acid, such as formic acid. The cilexetil trityl candesartan is heated to reflux until a clear solution is obtained. Typically, the reaction temperature is from about 30° C. to about 90° C., preferably from about 50° C. to about 90° C., and the heating takes place for about 5 to about 19 hours, preferably for about 8 to about 12 hours. Thereafter, the solvents are removed by evaporation to obtain crude deprotected candesartan cilexetil. The solvents may be removed at a temperature of about 30° C. to about 70° C., preferably at a temperature of about 50° C., and at a reduce pressure of about 30 mbar.

후처리

  1. temperatureTypically, the deprotection step comprises heating
  2. temperatureto reflux until a clear solution
  3. customis obtained
  4. customis from about 30° C. to about 90° C., preferably from about 50° C. to about 90° C.
  5. customfor about 5 to about 19 hours
  6. waitpreferably for about 8 to about 12 hours
  7. customThereafter, the solvents are removed by evaporation

출처 및 근거

ORD 기록
ord-9ddc7e8714f848aa8be681a6021447c6
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098342B2

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