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1,1'-Carbonyldiimidazole → HCID 54559816, 화합물

HRID 863500
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HRID 863500 반응식
[C:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=O)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N1C=CN=C1)(N1C=CN=C1)=O.Cl.[NH2:30][CH:31]1[CH2:45][C:34]2[C:35]3[NH:36][C:37](=[O:44])[C:38](=[O:43])[NH:39][C:40]=3[CH:41]=[CH:42][C:33]=2[CH2:32]1>O1CCCC1>[C:4]([O:3][C:1]([N:8]1[CH2:9][CH2:10][CH:11]([C:14](=[O:16])[NH:30][CH:31]2[CH2:45][C:34]3[C:35]4[NH:36][C:37](=[O:44])[C:38](=[O:43])[NH:39][C:40]=4[CH:41]=[CH:42][C:33]=3[CH2:32]2)[CH2:12][CH2:13]1)=[O:2])([CH3:5])([CH3:6])[CH3:7]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 682631,1'-CarbonyldiimidazoleHCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acidHCID 19696185HCID 19696185, 화합물

생성물 1

HCID 54559816HCID 54559816, 화합물수율 70%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

A mixture of N-Boc-piperidine-4-carboxylic acid (0.23 g, 1 mmol) and 1,1'-carbonyldiimidazole (0.16 g, 1 mmol) in tetrahydrofuran (5 mL) was heated at 80° C. for 15 min. After cooling, it was added to a solution of 8-amino-4,7,8,9-tetrahydro-1H-cyclopenta[f]quinoxaline-2,3-dione hydrochloride (0.11 g, 0.5 mmol) and the mixture was heated at 70° C. for 2 days. After filtration to remove precipitate, the filtrate was evaporated and the residue suspended in water. The resulting solid was collected by filtration, washed with diethyl and dried in vacuo (0.15 g, 70% yield).

후처리

  1. temperatureAfter cooling
  2. temperaturethe mixture was heated at 70° C. for 2 days
  3. filtrationAfter filtration
  4. customto remove precipitate
  5. customthe filtrate was evaporated
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with diethyl
  8. customdried in vacuo (0.15 g, 70% yield)

출처 및 근거

ORD 기록
ord-b34aa1eeb3da4d138021a5c26854f90a
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05721234

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