Dicyclohexylcarbodiimide → HCID 14182508、化合物

HRID 1252621ノート

反応式

HRID 1252621 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 14182508HCID 14182508、化合物収率 82.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-81ed4b1db5334fe3bea74590afbf00bf
出典データセット
uspto-grants-1988_05
特許番号
US04743685

反応ノート

読み込み中…