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

Dichloromethane → Ceftobiprole

HRID 1633813
노트
인쇄 미리보기

반응식

HRID 1633813 반응식
[NH2:1][C:2]1[S:6][N:5]=[C:4](/[C:7](=[N:42]/[O:43]C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)/[C:8]([NH:10][C@@H:11]2[C:18](=[O:19])[N:17]3[C@@H:12]2[S:13][CH2:14][C:15](/[CH:23]=[C:24]2/[C:25](=[O:41])[N:26]([C@@H:29]4[CH2:33][CH2:32][N:31](C(OC(C)(C)C)=O)[CH2:30]4)[CH2:27][CH2:28]/2)=[C:16]3[C:20]([OH:22])=[O:21])=[O:9])[N:3]=1.C1(OC)C=CC=CC=1.ClCCl.FC(F)(F)C(O)=O>C(O)=O.C1(C)C=CC=CC=1>[NH2:1][C:2]1[S:6][N:5]=[C:4](/[C:7](=[N:42]/[OH:43])/[C:8]([NH:10][C@@H:11]2[C:18](=[O:19])[N:17]3[C@@H:12]2[S:13][CH2:14][C:15](/[CH:23]=[C:24]2/[C:25](=[O:41])[N:26]([C@@H:29]4[CH2:33][CH2:32][NH:31][CH2:30]4)[CH2:27][CH2:28]/2)=[C:16]3[C:20]([OH:22])=[O:21])=[O:9])[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 12993648HCID 12993648, 화합물

생성물 1

HCID 135413542Ceftobiprole수율 80.4%

시약·촉매·용매 2

HCID 284Formic Acid용매
HCID 1140Toluene용매

반응 조건

온도
30 °C

실험 절차

5.1 (small scale): A suspension of 149 mg of (6R,7R)-7-[(Z)-2-(5-amino-[1,2,4]thiadiazol-3-yl)-2-trityloxyimino-acetylamino]-3-[(E)-(R)-1′-tert.-butoxycarbonyl-2-oxo-[1,3′]bipyrrolidinyl-3-ylidene-methyl]-8-oxo-5-thia-1-aza-bicyclo[4.2.0]oct-2-ene-2-carboxylic acid and 0.24 ml of methyl phenyl ether in 0.8 ml of formic acid was treated with 0.26 ml of dichloromethane containing 2% of trifluoroacetic acid and the solution was heated to 30° C. for 3 h after which time HPLC indicated completion of the reaction. The mixture was diluted with 3 ml of toluene and evaporated to dryness. The residue was diluted with 2 ml of methanol and 6 ml of water, the pH was adjusted to 9 by adding diluted ammonia and the aqueous layer was washed three times with ethyl acetate. The pH of the aqueous layer was adjusted to 3 by adding diluted hydrochloric acid and the solution was evaporated to dryness. The residue was digested with t-butyl methyl ether, filtered and the residue dried to give 73 mg of the NMR-pure title compound as a pale yellow solid. 1H-NMR (d6-DMSO+1 equivalent of CF3COOH, only some selected signals given): 7.26 (s, 1H, CH—C(3)); 5.88 (d, J=4.8, 1H, H—C(7)); 5.18 (d, J=4.8, 1H, H—C(6)); 3.88 and 3.86 (d each, J=18 each, 2H, CH2—S(5)); 3.5-2.8 (m, 8H, 4×CH2); 2.2-2.0 (m, 2H, CH2).

후처리

  1. customcompletion of the reaction
  2. customevaporated to dryness
  3. additionThe residue was diluted with 2 ml of methanol and 6 ml of water
  4. additionby adding diluted ammonia
  5. washthe aqueous layer was washed three times with ethyl acetate
  6. additionby adding diluted hydrochloric acid
  7. customthe solution was evaporated to dryness
  8. filtrationfiltered
  9. customthe residue dried

출처 및 근거

ORD 기록
ord-4c2331eb421a4fceb37d30f2594d4e1c
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06504025B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트