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

Dimethylformamide → HCID 86752547, 화합물

HRID 1289779
노트
인쇄 미리보기

반응식

HRID 1289779 반응식
[NH2:1][C:2]1[N:6]=[C:5]([NH2:7])[N:4]([C:8]([NH:10][CH3:11])=[S:9])[N:3]=1.CN(C)[CH:14]=[O:15].[CH2:17](N(CC)CC)C.CC[C:26]([C:28](Cl)=[O:29])=[O:27]>O.C(Cl)(Cl)Cl>[NH2:7][C:5]1[N:4]([C:8]([NH:10][CH3:11])=[S:9])[N:3]=[C:2]([NH:1][C:26]([C:28]([O:15][CH2:14][CH3:17])=[O:29])=[O:27])[N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 10725863HCID 10725863, 화합물HCID 11007880Butanoyl chloride, 2-oxo-

생성물 1

HCID 86752547HCID 86752547, 화합물수율 19%

시약·촉매·용매 2

HCID 962Water용매
HCID 6212
Chloroform
용매

실험 절차

The compound (4.00 g) obtained in Example 31, dimethylformamide (80 ml) and triethylamine (3.9 ml) were cooled to 0° C. Ethyloxalyl chloride (2.7 ml) was gradually added dropwise and the mixture was stirred at 0° C.-room temperature for 2.5 hours. After the stirring, chloroform (50 ml) was added and the mixture was stirred at 0° C. for 30 minutes. The reaction mixture was poured into water and extracted with chloroform. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure to give a pale-yellow liquid. This liquid was subjected to silica gel column chromatography (chloroform-methanol) and recrystallization from ethanol to give 1.22 g of white powdery crystals (yield 19%).

후처리

  1. stirringthe mixture was stirred at 0° C. for 30 minutes
  2. extractionextracted with chloroform
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled away under reduced pressure
  6. customto give a pale-yellow liquid
  7. customThis liquid was subjected to silica gel column chromatography (chloroform-methanol) and recrystallization from ethanol

출처 및 근거

ORD 기록
ord-6954eba5541e4d9db465f6ba146872f2
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05750545

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트