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

Hydrochloric Acid → 2-(3-chloro-4,5-dihydro-1,2-oxazol-5-yl)-2-(9H-fluoren-9-ylmethoxycarbonylamino)acetic acid

HRID 543451
노트
인쇄 미리보기

반응식

HRID 543451 반응식
[CH2:1]1[C:5]([Cl:6])=[N:4][O:3][C@@H:2]1[C@H:7]([NH2:11])[C:8]([OH:10])=[O:9].[C:12](=[O:15])(O)[O-:13].[Na+].O[CH2:18][CH:19]1[C:31]2[C:30](C(Cl)=O)=[CH:29][CH:28]=[CH:27][C:26]=2[C:25]2[C:20]1=[CH:21][CH:22]=[CH:23][CH:24]=2.Cl>C(OCC)(=O)C.O>[Cl:6][C:5]1[CH2:1][CH:2]([CH:7]([NH:11][C:12]([O:13][CH2:18][CH:19]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:25]=3[C:26]3[C:31]2=[CH:30][CH:29]=[CH:28][CH:27]=3)=[O:15])[C:8]([OH:10])=[O:9])[O:3][N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 294641AcivicinHCID 516892Sodium BicarbonateHCID 86737604HCID 86737604, 화합물

생성물 1

HCID 3323662-(3-chloro-4,5-dihydro-1,2-oxazol-5-yl)-2-(9H-fluoren-9-ylmethoxycarbonylamino)acetic acid

시약·촉매·용매 2

HCID 962Water
용매
HCID 8857Ethyl Acetate용매

실험 절차

To 178 mg. of AT-125 in 4 ml. of water is added 300 mg. of sodium bicarbonate. After cooling the mixture to 0°-5° C., 300 mg. of 9-hydroxymethyl fluorenylcarbonyl chloride is added and it is stirred for two hours and allowed to stand overnight at room temperature. The resulting semi solid is taken up in ethyl acetate and 1 N hydrochloric acid is added until a pH of 3 is attained. The organic phase is separated, dried over sodium sulfate, concentrated and chromatographed on 20 g. of CC-4 silica gel employing 40% ethyl acetate/Hexane. Those fractions containing the desired product are evaporated and the residue recrystallized from ethyl acetate to yield 3-chloro-α-[[(9H-fluoren-9-yl-methoxy)carbonyl]amino]-4,5-dihydro-5-isoxazole acetic acid, m.p. 182°-183° C. The NMR fits the desired structure.

후처리

  1. temperatureAfter cooling the mixture to 0°-5° C.
  2. waitto stand overnight at room temperature
  3. customThe organic phase is separated
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customchromatographed on 20 g
  7. additionThose fractions containing the desired product
  8. customare evaporated
  9. customthe residue recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-479aa39202df46b2a3d4f511ff4543e1
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE031578

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트