홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → Pentanoic acid [6-benzyl-4-(2-chloro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amide

HRID 1020007
노트
인쇄 미리보기

반응식

HRID 1020007 반응식
CO[C:3]([CH:5]1[C:10](=O)[CH2:9][CH2:8][N:7]([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:6]1)=O.[ClH:19].[NH2:20][C:21]([NH2:23])=[NH:22].[C:24](=[O:27])([O-])[O-].[K+].[K+].O>CN(C=O)C.CO>[CH2:12]([N:7]1[CH2:8][CH2:9][C:10]2[N:22]=[C:21]([NH:23][C:24](=[O:27])[CH2:3][CH2:5][CH2:10][CH3:9])[N:20]=[C:3]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:5]=2[CH2:6]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 107480Methyl 1-benzyl-4-oxo-3-piperidinecarboxylate

생성물 1

HCID 46937260Pentanoic acid [6-benzyl-4-(2-chloro-phenyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl]-amide수율 87%

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 6228Dimethylformamide용매

실험 절차

Methyl-1-benzyl-4-oxo-3-piperidine carboxylate (5.68 g., 20 mmoles) and guanidine hydrochloride (2.0 g., 21 mmoles) were suspended and stirred in dry DMF (45 mls) before potassium carbonate (5.68 g., 41 mmoles) was added portionwise over 15 minutes. The reaction mixture was poured onto cold water (750 mls) to release a white/beige solid which was rapidly stirred for 30 minutes. The solid was filtered washed with water (100 mls) and dried in a vacuum desiccator. The product was then slurried in ether (150 mls), filtered and dried in vacuo overnight, to leave an off-white solid (4.46 g., 87% yield). Single spot by tlc (MeOH, Rf 0.66), LC-MS (retention 2.20 mins., mass 257 M+H).

후처리

  1. additionwas added portionwise over 15 minutes
  2. filtrationThe solid was filtered
  3. washwashed with water (100 mls)
  4. customdried in a vacuum desiccator
  5. filtrationfiltered
  6. customdried in vacuo overnight
  7. customto leave an off-white solid (4.46 g., 87% yield)

출처 및 근거

ORD 기록
ord-52fae9d42e2e45bc97532e3e142d46a0
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716302B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트