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Potassium Phosphate, Tribasic → 5-(4-(3-Chlorophenoxy)-3-methoxyphenyl)-7-(3-methoxyphenyl)-6-(3-(pyrrolidin-1-yl)propyl)pyrrolo[2,1-f][1,2,4]triazin-4-amine

HRID 1615466
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인쇄 미리보기

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HRID 1615466 반응식
Br[C:2]1[C:3]([CH2:20][CH2:21][CH2:22][N:23]2[CH2:27][CH2:26][CH2:25][CH2:24]2)=[C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[CH:13]=2)[N:5]2[C:10]=1[C:9]([NH2:11])=[N:8][CH:7]=[N:6]2.[Cl:28][C:29]1[CH:30]=[C:31]([CH:44]=[CH:45][CH:46]=1)[O:32][C:33]1[CH:38]=[CH:37][C:36](B(O)O)=[CH:35][C:34]=1[O:42][CH3:43].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>CN(C=O)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>[Cl:28][C:29]1[CH:30]=[C:31]([CH:44]=[CH:45][CH:46]=1)[O:32][C:33]1[CH:38]=[CH:37][C:36]([C:2]2[C:3]([CH2:20][CH2:21][CH2:22][N:23]3[CH2:27][CH2:26][CH2:25][CH2:24]3)=[C:4]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[CH:13]=3)[N:5]3[C:10]=2[C:9]([NH2:11])=[N:8][CH:7]=[N:6]3)=[CH:35][C:34]=1[O:42][CH3:43]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 66601935HCID 66601935, 화합물HCID 706646535-Bromo-7-(3-methoxyphenyl)-6-(3-(pyrrolidin-1-yl)propyl)pyrrolo[2,1-f][1,2,4]triazin-4-amine

생성물 1

HCID 497875755-(4-(3-Chlorophenoxy)-3-methoxyphenyl)-7-(3-methoxyphenyl)-6-(3-(pyrrolidin-1-yl)propyl)pyrrolo[2,1-f][1,2,4]triazin-4-amine수율 41.1%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

To a solution of the compound (43 mg, 0.01 mmol) prepared in Example 15, the compound (29.4 mg, 0.15 mmol) prepared in Example 10, potassium phosphate (2N, 0.1 mL, 0.2 mmol), Pd(PPh3)4 (3 mg, 0.003 mmol) in DMF (3 mL) was deoxygenated by nitrogen gas for 5 minutes, and the reactor was sealed, heated at 90° C. for 6 hours. The mixture was concentrated, purified by prep TLC using 5% methanol in DCM (with 3% ammonium hydroxide solution) to give crude product which was further purified by prep HPLC to obtain the title compound (2.4 mg) having the following physical data.

후처리

  1. customthe reactor was sealed
  2. concentrationThe mixture was concentrated
  3. custompurified by prep TLC
  4. customto give crude product which
  5. customwas further purified by prep HPLC

출처 및 근거

ORD 기록
ord-e3bdc3a7c32b420fa80f0dd29117f631
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765754B2

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