Dicyclohexylcarbodiimide → HCID 14182508, 화합물

HRID 1252621

반응식

HRID 1252621 반응식
[C:1]1([CH2:7][O:8][C:9]2[C:14]([O:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[CH:13][N:12]=[C:11]([C:23]([OH:25])=O)[CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.OC1C2N=NNC=2C=CC=1.[NH2:36][N:37]1[CH2:42][CH2:41][NH:40][C:39](=[O:43])[C:38]1=[O:44].C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C=O>[O:44]=[C:38]1[C:39](=[O:43])[NH:40][CH2:41][CH2:42][N:37]1[NH:36][C:23]([C:11]1[CH:10]=[C:9]([O:8][CH2:7][C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:14]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:13][N:12]=1)=[O:25]

참가 물질

6

반응물 4

HCID 10868DicyclohexylcarbodiimideHCID 141825074,5-bis(phenylmethoxy)-2-Pyridinecarboxylic acidHCID 221847681-Aminopiperazine-2,3-dioneHCID 178418300HCID 178418300, 화합물

생성물 1

HCID 14182508HCID 14182508, 화합물수율 82.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 4,5-bis(phenylmethoxy)-2-pyridinecarboxylic acid (7.1 g, 21.17 mmol), hydroxybenzotriazole (0.29 g, 2.12 mmol) and N-aminopiperazine-2,3-dione (2.73 g, 21.17 mmol) in 140 ml of dry dimethylformamide was added, after 15 minutes of stirring, 4.80 g (23.3 mmol) of dicyclohexylcarbodiimide. After stirring for 21 hours at room temperature, dicyclohexylurea was filtered off (4.0 g ) and the solvent was evaporated in vacuo. The solid residue was triturated for 40 minutes with 240 ml of tetrahydrofuran, filtered, washed with tetrahyrofuran and dried in vacuo to yield 7.76 g of the title compound, melting point 231.1° C.

후처리

  1. additionwas added, after 15 minutes
  2. stirringAfter stirring for 21 hours at room temperature
  3. filtrationdicyclohexylurea was filtered off (4.0 g )
  4. customthe solvent was evaporated in vacuo
  5. customThe solid residue was triturated for 40 minutes with 240 ml of tetrahydrofuran
  6. filtrationfiltered
  7. washwashed with tetrahyrofuran
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-81ed4b1db5334fe3bea74590afbf00bf
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04743685

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