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

1,2,4-Trimethylbenzene → HCID 86701346, 화합물

HRID 2179847
노트
인쇄 미리보기

반응식

HRID 2179847 반응식
[C:1]1([C:11]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:18](B(O)O)=[C:17]3[C:12]=2[CH:13]=[CH:14][CH:15]=[CH:16]3)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.FC(F)(F)S(O[C:34]1[CH:43]=[CH:42][C:41]2[C:36](=[CH:37][C:38]([O:44][CH3:45])=[CH:39][CH:40]=2)[CH:35]=1)(=O)=O.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C1(C(=CC(=CC=1)C)C)C>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.O.CC(O)C>[CH3:45][O:44][C:38]1[CH:37]=[C:36]2[C:41]([CH:42]=[CH:43][C:34]([C:18]3[C:17]4[C:12]([C:11]([C:1]5[C:10]6[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=6)[CH:4]=[CH:3][CH:2]=5)=[C:24]5[C:19]=3[CH:20]=[CH:21][CH:22]=[CH:23]5)=[CH:13][CH:14]=[CH:15][CH:16]=4)=[CH:35]2)=[CH:40][CH:39]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 72471,2,4-TrimethylbenzeneHCID 62657Potassium Phosphate, TribasicHCID 10892112Methanesulfonic acid, trifluoro-, 7-methoxy-2-naphthalenyl esterHCID 23088558[10-(Naphthalen-1-yl)anthracen-9-yl]boronic acid

생성물 1

HCID 86701346HCID 86701346, 화합물수율 52.7%

시약·촉매·용매 3

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 962Water용매2회
HCID 3776Isopropanol용매

실험 절차

Under the nitrogen atmosphere, (10-(naphthalen-1-yl)anthracen-9-yl)boronic acid (25.1 g), 7-methoxynaphthalen-2-yl trifluoromethane sulfonate (24.3 g), Pd(PPh3)4 (0.9 g), potassium phosphate (30.6 g), and a mixture solvent (260 ml) of pseudo cumene, IPA, and water (pseudo cumene/IPA/water=8/4/1 (volume ratio)) were added to a flask and refluxed for 4.5 hours. Once the heating is completed, water was added. After cooling to room temperature, a solid was collected by suction filtration. The obtained solid was washed with water and subsequently with methanol, dissolved in toluene, and purified with a silica gel short column. Crystals obtained by slow distillation of the solvent under reduced pressure were collected by suction filtration to give 9-(7-methoxynaphthalen-2-yl)-10-(naphthalen-1-yl)anthracene (17.5 g) as a third intermediate compound. The scheme is shown in the following “Reaction 4”.

후처리

  1. temperaturerefluxed for 4.5 hours
  2. filtrationa solid was collected by suction filtration
  3. washThe obtained solid was washed with water and subsequently with methanol
  4. dissolutiondissolved in toluene
  5. custompurified with a silica gel short column
  6. customCrystals obtained by slow distillation of the solvent under reduced pressure
  7. filtrationwere collected by suction filtration

출처 및 근거

ORD 기록
ord-046678364a4646ae9a449b0b6bb6b3d4
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09070885B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트