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

Potassium Carbonate → HCID 86705363, 화합물

HRID 1773659
노트
인쇄 미리보기

반응식

HRID 1773659 반응식
[Br:1][C:2]1[CH:3]=[C:4](Br)[C:5]2[N:6]([C:8](I)=[CH:9][N:10]=2)[N:7]=1.CCN(C(C)C)C(C)C.[N:22]1([CH2:28][CH2:29][NH2:30])[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1.[CH3:31][C:32]1[CH:33]=[C:34](B(O)O)[CH:35]=[CH:36][C:37]=1[C:38](=[O:41])[NH:39][CH3:40].C(=O)([O-])[O-].[K+].[K+]>CN1C(=O)CCC1.C1COCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([NH:30][CH2:29][CH2:28][N:22]2[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)[C:5]2[N:6]([C:8]([C:34]3[CH:35]=[CH:36][C:37]([C:38]([NH:39][CH3:40])=[O:41])=[C:32]([CH3:31])[CH:33]=3)=[CH:9][N:10]=2)[N:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 4082852-MorpholinoethylamineHCID 66691681HCID 66691681, 화합물HCID 86705359HCID 86705359, 화합물

생성물 1

HCID 86705363HCID 86705363, 화합물

시약·촉매·용매 4

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매
HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
70 °C

실험 절차

To a stirred solution of 2.01 g (5 mmol) 6,8-dibromo-3-iodoimidazo[1,2-b]pyridazine which was prepared according to intermediate example 96c in NMP (15 mL) were added 1.94 g (15 mmol) DIPEA and 1.30 g (10 mmol) 2-(morpholin-4-yl)ethanamine in one portion at rt. After heating for 2 h at 70° C., 100 mL DCM were added and the mixture was washed with water (3×100 mL). The organic phase was dried over sodium sulphate and evaporated to yield a brownish solid which was used without further purification in the next step. To a stirred solution of the remaining solid in 20 mL THF were added 1.16 g (6 mmol) [3-methyl-4-(methylcarbamoyl)phenyl]boronic acid which was prepared according to intermediate example 562b, 15 mL aqueous potassium carbonate solution (15 mmol, 1M), 816 mg Pd(dppf)Cl2 (1 mmol) and the mixture was heated for 41 h at 70° C., to yield after working up and purification 2.35 g (99%) of the title compound.

후처리

  1. washthe mixture was washed with water (3×100 mL)
  2. dry with materialThe organic phase was dried over sodium sulphate
  3. customevaporated
  4. customto yield a brownish solid which
  5. customwas used without further purification in the next step
  6. customwas prepared
  7. temperaturethe mixture was heated for 41 h at 70° C.
  8. customto yield
  9. custompurification 2.35 g (99%) of the title compound

출처 및 근거

ORD 기록
ord-e43fa7be1a60476cb17dc9d3c50c88fe
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09255100B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트