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

Ammonia → 3-(2,3beta-Dihydro-6-methyl-1-methylthio-13-nitro-8alpha-ergolinyl)-1,1-diethylurea

HRID 1073301
노트
인쇄 미리보기

반응식

HRID 1073301 반응식
[CH3:1][N:2]1[C@H:16]2[C@@H:6]([C:7]3[CH:8]=[C:9]([N+:18]([O-:20])=[O:19])[CH:10]=[C:11]4[C:17]=3[C@H:14]([CH2:15]2)[CH2:13][NH:12]4)[CH2:5][C@H:4]([NH:21][C:22](=[O:28])[N:23]([CH2:26][CH3:27])[CH2:24][CH3:25])[CH2:3]1.F[B-](F)(F)F.[CH3:34][S+:35](C)SC.N>O1CCCC1>[CH3:1][N:2]1[C@H:16]2[C@@H:6]([C:7]3[CH:8]=[C:9]([N+:18]([O-:20])=[O:19])[CH:10]=[C:11]4[C:17]=3[C@H:14]([CH2:15]2)[CH2:13][N:12]4[S:35][CH3:34])[CH2:5][C@H:4]([NH:21][C:22](=[O:28])[N:23]([CH2:26][CH3:27])[CH2:24][CH3:25])[CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 2737114Dimethyl(methylthio)sulfonium TetrafluoroborateHCID 13374954HCID 13374954, 화합물

생성물 1

HCID 867443363-(2,3beta-Dihydro-6-methyl-1-methylthio-13-nitro-8alpha-ergolinyl)-1,1-diethylurea수율 64.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Under argon, 38 mg (0.1 mmol) of 3-(2,3β-dihydro-6-methyl-13-nitro-8α-ergolinyl)-1,1-diethylurea in 2 ml of absolute, freshly distilled tetrahydrofuran is combined with 47 mg (0.24 mmol) of dimethylmethylthiosulfonium fluoroborate, and the mixture is agitated for 20 minutes at room temperature. For working-up purposes, the batch is poured on 10 ml of ice and rendered alkaline with 25% strength ammonia solution. The organic phase is extracted repeatedly with methylene chloride. The extracts are dried over magnesium sulfate and concentrated. The crude product is purified over a preparative silica gel plate with methylene chloride/methanol 9:1 as the eluent, thus obtaining 28 mg of 3-(2,3β-dihydro-6-methyl-1-methylthio-13-nitro-8α-ergolinyl)-1,1-diethylurea.

후처리

  1. extractionThe organic phase is extracted repeatedly with methylene chloride
  2. dry with materialThe extracts are dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe crude product is purified over a preparative silica gel plate with methylene chloride/methanol 9:1 as the eluent

출처 및 근거

ORD 기록
ord-f4a2097aca7741f9ba087216961d9533
출처 데이터셋
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04968801

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트