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

2-Bromo-6-(1,3-dioxolan-2-yl)pyridine → 2-Cyclopropyl-6-(1,3-dioxolan-2-yl)pyridine

HRID 2220069
노트
인쇄 미리보기

반응식

HRID 2220069 반응식
[CH:1]1([Mg]Br)[CH2:3][CH2:2]1.Br[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH:13]2[O:17][CH2:16][CH2:15][O:14]2)[N:8]=1>C1COCC1.[Cl-].[Zn+2].[Cl-].[O-]S([O-])(=O)=O.[Zn+2].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([CH:13]3[O:14][CH2:15][CH2:16][O:17]3)[N:8]=2)[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 1186132-Bromo-6-(1,3-dioxolan-2-yl)pyridineHCID 178418630HCID 178418630, 화합물

생성물 1

HCID 193617732-Cyclopropyl-6-(1,3-dioxolan-2-yl)pyridine수율 93%

시약·촉매·용매 4

HCID 24424Zinc Sulfate촉매HCID 3007855Zincchloride촉매
HCID 178418397
HCID 178418397, 화합물
촉매
HCID 8028Tetrahydrofuran용매3회

실험 절차

To a stirred solution of 0.5 M zinc chloride in THF (9.1 mL, 4.55 mmol) under N2, cooled to −78° C. was added dropwise a solution of 0.5 M cyclopropylmagnesium bromide in THF (9.1 mL, 4.55 mmol). The reaction mixture was warmed to RT and stirred for 1 h. The resulting zincate was transferred via syringe to a sealed tube containing a solution of 2-bromo-6-(1,3-dioxolan-2-yl)pyridine of Step B (694.3 mg, 3.03 mmol) and Pd(PPh3)4 in dry THF (3 mL). The reaction mixture was degassed, sealed and heated at 120° C. for 2 h. The reaction mixture was cooled to RT and partitioned between ethyl acetate (100 mL) and saturated aqueous NH4Cl (50 mL). The phases were separated. The aqueous phase was extracted with ethyl acetate (15 mL). The combined organic phases were dried (MgSO4), filtered and concentrated. The resulting residue was dissolved in CH2Cl2, adsorbed onto silica gel and purified on a Biotage 40S column with SIM using 10% ethyl acetate in hexane as the eluent to afford 538.2 mg (2.82 mmol, 93%) of the desired product as a bright yellow liquid.

후처리

  1. customThe reaction mixture was degassed
  2. customsealed
  3. temperatureheated at 120° C. for 2 h
  4. temperatureThe reaction mixture was cooled to RT
  5. custompartitioned between ethyl acetate (100 mL) and saturated aqueous NH4Cl (50 mL)
  6. customThe phases were separated
  7. extractionThe aqueous phase was extracted with ethyl acetate (15 mL)
  8. dry with materialThe combined organic phases were dried (MgSO4)
  9. filtrationfiltered
  10. concentrationconcentrated
  11. dissolutionThe resulting residue was dissolved in CH2Cl2
  12. custompurified on a Biotage 40S column with SIM

출처 및 근거

ORD 기록
ord-9ea9c2e04e89462394c3858924ada901
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07417041B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트