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

Nitrate → HCID 178418760, 화합물

HRID 11865
노트
인쇄 미리보기

반응식

HRID 11865 반응식
[NH2:1][CH2:2][C:3]1[CH:34]=[CH:33][C:6]([C:7]([NH:9][C@@H:10]([CH2:14][CH2:15][CH2:16][CH2:17][N:18]([CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=2)C(OC(C)(C)C)=O)[C:11]([OH:13])=[O:12])=[O:8])=[CH:5][CH:4]=1.[N+:35]([O-])([O-])=O.C([N:41]([CH2:44]C)CC)C>CN(C=O)C>[NH:1]([CH2:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([NH:9][C@@H:10]([CH2:14][CH2:15][CH2:16][CH2:17][NH:18][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=2)[C:11]([OH:13])=[O:12])=[O:8])=[CH:33][CH:34]=1)[C:44]([NH2:41])=[NH:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 943NitrateHCID 8471TriethylamineHCID 21043758(S)-2-((4-aminomethylbenzoyl)amino)-5-(N-Boc-2-picolylaminomethyl)valeric Acid

생성물 1

HCID 178418760HCID 178418760, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The compound obtained in Example 41-5 (0.01 g) was dissolved in DMF (0.3 ml). After the addition of dimethylpyrazolecarboxyamidine nitrate (0.01 g), the mixture was adjusted to pH 8 with triethylamine and stirred for 3 days. The reaction solution was concentrated. Chloroform was added to the residue and the mixture was washed with saturated aqueous solution of sodium hydrogencarbonate. The organic layer was concentrated and dried under reduced pressure. The residue was purified by silica gel column chromatography (5 g, chloroform/methanol/water=7/3/0.5) to obtain the title compound (0.01 g) as white foam. The foam was dissolved in methanol (0.3 ml) and 4 mol/l hydrochloric acid/dioxane solution (0.3 ml) was added dropwise. The mixture was stirred for 3 hours at room temperature. The reaction solution was concentrated and dried under reduced pressure to obtain a crude product (0.01 g). The crude product was purified by silica gel column chromatography (0.5 g, chloroform/methanol/water=7/3/0.5) and 1 mol/l hydrochloric acid was added. The mixture was concentrated to obtain hydrochloride of the title compound (0.01 g) as white foam.

후처리

  1. concentrationThe reaction solution was concentrated
  2. additionChloroform was added to the residue
  3. washthe mixture was washed with saturated aqueous solution of sodium hydrogencarbonate
  4. concentrationThe organic layer was concentrated
  5. customdried under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (5 g, chloroform/methanol/water=7/3/0.5)

출처 및 근거

ORD 기록
ord-1b8da72fa0b543b09dd1bd7a4a052cdb
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07098215B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트