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

Hydrochloric Acid → 3-[4-(Cyclopropyl-methyl-amino)-5,6,7,8-tetrahydro-[1]benzothiopheno[2,3-d]pyrimidin-2-yl]-propionic acid

HRID 1056843
노트
인쇄 미리보기

반응식

HRID 1056843 반응식
[Li+].[OH-].C[O:4][C:5](=[O:26])[CH2:6][CH2:7][C:8]1[N:9]=[C:10]([N:21]([CH:23]2[CH2:25][CH2:24]2)[CH3:22])[C:11]2[C:16]3[CH2:17][CH2:18][CH2:19][CH2:20][C:15]=3[S:14][C:12]=2[N:13]=1.Cl>O.C1COCC1>[CH:23]1([N:21]([CH3:22])[C:10]2[C:11]3[C:16]4[CH2:17][CH2:18][CH2:19][CH2:20][C:15]=4[S:14][C:12]=3[N:13]=[C:8]([CH2:7][CH2:6][C:5]([OH:26])=[O:4])[N:9]=2)[CH2:24][CH2:25]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 897192803-[4-(Cyclopropyl-methyl-amino)-5,6,7,8-tetrahydro-[1]benzothiopheno[2,3-d]pyrimidin-2-yl]-propionic acid methyl ester

생성물 1

HCID 716677593-[4-(Cyclopropyl-methyl-amino)-5,6,7,8-tetrahydro-[1]benzothiopheno[2,3-d]pyrimidin-2-yl]-propionic acid수율 54%

시약·촉매·용매 2

HCID 962
Water
용매
2회
HCID 8028Tetrahydrofuran용매

실험 절차

The LiOH (0.047 g, 0.0018 mol) dissolved in water (2 ml) was added to a solution of 3-[4-(cyclopropyl-methyl-amino)-5,6,7,8-tetrahydro-[1]benzothiopheno[2,3-d]pyrimidin-2-yl]-propionic acid methyl ester (0.5 g, 0.0014 mol) in THF (3 ml), and the resulting solution was stirred at R.T for 3 hrs. The reaction mixture was diluted with water, acidified with dilute HCl (up to pH 5) and extracted with ethyl acetate (3×15 ml). The combined organic layers were dried over Na2SO4, concentrated, and the crude was purified by preparative HPLC to give 0.25 g (54%) of 3-[4-(cyclopropyl-methyl-amino)-5,6,7,8-tetrahydro-[1]benzothiopheno[2,3-d]pyrimidin-2-yl]-propionic acid. 1H NMR (400 MHz, CDCl3) δ ppm=0.53 (m, 2H), 0.87 (m, 2H), 1.76 (m, 2H), 1.92 (m, 2H), 2.84 (m, 7H), 3.1 (s, 3H), 3.22 (t, 2H), 14.75 (s, 1H). LC-MS: [M+H]=331.9.

후처리

  1. extractionextracted with ethyl acetate (3×15 ml)
  2. dry with materialThe combined organic layers were dried over Na2SO4
  3. concentrationconcentrated
  4. customthe crude was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-6e3c6c5c45b446c49aba85104af4286a
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09399647B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트