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

1,1-Dibromoethane → Benzyl 3-phenylpropanoate

HRID 1594655
노트
인쇄 미리보기

반응식

HRID 1594655 반응식
BrC(Br)C.[CH2:5]([O:12][C:13](=[O:25])[C@H:14]([CH3:24])N(I)C(OC(C)(C)C)=O)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.I[C:27]1[CH:32]=[CH:31][C:30](C2(C([O-])=O)CC2)=[CH:29][CH:28]=1.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C>C1COCC1.CC(N(C)C)=O.C(OCC)(=O)C.[Zn].C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH2:5]([O:12][C:13](=[O:25])[CH2:14][CH2:24][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 112011,1-DibromoethaneHCID 80271Tri-o-tolylphosphineHCID 21968199N-Boc-iodo-L-alanine benzyl esterHCID 863308141-(4-Iodophenyl)cyclopropane-1-carboxylate

생성물 1

HCID 562789Benzyl 3-phenylpropanoate수율 67.1%

시약·촉매·용매 5

HCID 23994
Zinc
촉매
HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매
HCID 31374Dimethylacetamide용매2회

반응 조건

온도
55 °C

실험 절차

A suspension of zinc (0.874 g) in THF with dibromoethane (0.02 mL) was sonicated at 40° C. for 40 minutes under argon. N-Boc-iodo-L-alanine benzyl ester (4.20 g, 10.4 mmol) and dimethylacetamide (5 mL) were added, and the mixture was heated at 55° C. for 1 hour. tbutyl 1-(4-iodophenyl)cyclopropane-1-carboxylate (3.26 g, 9.48 mmol) in dimethylacetamide (10 mL) was added followed by tris(dibenzylideneacetone)dipalladium(0) (0.33 g) and tri-o-tolylphosphine (0.398 g). Heating was continued under argon for 16 hours. The mixture was diluted with ethyl acetate, washed with water, dried, filtered and evaporated. Chromatography of the residue over silica gel (methylene chloride/hexane 1/3 to methylene chloride/ethyl acetate 95/5) gave 2-(S)-tbutoxycarbonylamino-3-[4′-1″-tbutoxycarbonyl)cyclopropyl]benzenepropanoic acid benzyl ester (3.15 g, 6.36 mmol, 67%).

후처리

  1. customwas sonicated at 40° C. for 40 minutes under argon
  2. temperatureHeating
  3. washwashed with water
  4. customdried
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-ac383dfc05024e9b8a6d92147fbc163f
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06284768B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트