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

Chloroacetyl chloride → 4-(2-chloroacetyl)-1H-pyrrole-2-carbaldehyde

HRID 1494415
노트
인쇄 미리보기

반응식

HRID 1494415 반응식
[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[O:7].[Cl-].[Al+3].[Cl-].[Cl-].[Cl:12][CH2:13][C:14](Cl)=[O:15]>ClC(Cl)C>[CH:6]([C:2]1[NH:1][CH:5]=[C:4]([C:14](=[O:15])[CH2:13][Cl:12])[CH:3]=1)=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6577Chloroacetyl chlorideHCID 13854Pyrrole-2-carboxaldehydeHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 27634524-(2-chloroacetyl)-1H-pyrrole-2-carbaldehyde수율 94%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

A mixture of 35 g (0.37 mole) pyrrole-2-carboxaldehyde in 325 ml dichloroethane was stirred under nitrogen in a three-necked, one-liter, round-bottomed flask fitted with an overhead stirrer and addition funnel. To this was added, in portions over a one-hour period, 294 g (2.21 mole) aluminum chloride. After the addition was completed, the mixture was stirred at room temperature for 10 minutes, then 124.7 g (88 ml, 1.10 mole) of chloroacetyl chloride was added dropwise over a one-hour period. The mixture was stirred at room temperature for 16 hours, then carefully poured into one liter of ice-water. The resulting precipitate (purple) was collected, washed well with water, and dried in vacuo. The dry solid was placed in a Soxhlet extractor and extracted with ethyl acetate for 20 hours. Concentration of the ethyl acetate solution afforded 59.4 g (94%) of the title compound as a yellow-green solid; m.p. 178°-179° C. This intermediate was used immediately in the next step. An analytical sample could be prepared by recrystallization from acetone.

후처리

  1. customfitted with an overhead stirrer and addition funnel
  2. additionTo this was added, in portions over a one-hour period
  3. additionAfter the addition
  4. stirringthe mixture was stirred at room temperature for 10 minutes
  5. stirringThe mixture was stirred at room temperature for 16 hours
  6. customThe resulting precipitate (purple) was collected
  7. washwashed well with water
  8. customdried in vacuo
  9. extractionextracted with ethyl acetate for 20 hours

출처 및 근거

ORD 기록
ord-c1002e677caa44f3a8840ae634ffae5f
출처 데이터셋
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05026715

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트