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

Nitrogen → 2-Methanesulfonyloxymethyl-oxazole-4-carboxylic acid ethyl ester

HRID 1189388
노트
인쇄 미리보기

반응식

HRID 1189388 반응식
N#N.[CH2:3]([O:5][C:6]([C:8]1[N:9]=[C:10]([CH2:13][OH:14])[O:11][CH:12]=1)=[O:7])[CH3:4].CCN(CC)CC.[S:22](Cl)([CH3:25])(=[O:24])=[O:23]>C(Cl)Cl.CN(C1C=CN=CC=1)C>[CH2:3]([O:5][C:6]([C:8]1[N:9]=[C:10]([CH2:13][O:14][S:22]([CH3:25])(=[O:24])=[O:23])[O:11][CH:12]=1)=[O:7])[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 947NitrogenHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 10511369Ethyl 2-(hydroxymethyl)oxazole-4-carboxylate

생성물 1

HCID 866649112-Methanesulfonyloxymethyl-oxazole-4-carboxylic acid ethyl ester

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine
촉매
HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 2-hydroxymethyl-oxazole-4-carboxylic acid ethyl ester (345 mg, 2.02 mmol) in dry CH2Cl2 (10 mL) was treated at 0° C. with Et3N (0.40 mL, 2.87 mmol) followed by DMAP (25 mg, 0.20 mmol) and Ms-Cl (0.20 mL, 2.60 mmol). After stirring at 0° C. for 2 h, the reaction was quenched with water (5 mL). The org. layer was dried over Na2SO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (1:2→1:1 EA-Hept) gave the title compound as a yellow solid. TLC: rf (1:1 EA-Hept)=0.23. LC-MS-conditions 01: tR=0.73 min; [M+H]+=249.94.

후처리

  1. customthe reaction was quenched with water (5 mL)
  2. dry with materiallayer was dried over Na2SO4
  3. filtrationfiltered
  4. customthe solvents were removed under reduced pressure
  5. customPurification of the residue by FC (1:2→1:1 EA-Hept)

출처 및 근거

ORD 기록
ord-476800d96fe441bbbee46117422a12d4
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08674111B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트