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Sodium Carbonate → HCID 59198487、化合物

HRID 1896533
ノート
印刷プレビュー

反応式

HRID 1896533 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]2[C:8]3[C:9]([NH:17][CH2:18][C:19]4[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=4)=[N:10][CH:11]=[C:12]([C:15]#[N:16])[C:13]=3[S:14][C:4]=2[CH:3]=1.[F:27][C:28]1[CH:33]=[CH:32][C:31](/[CH:34]=[CH:35]/B(O)O)=[CH:30][CH:29]=1.C([O-])([O-])=O.[Na+].[Na+].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>C(O)CC.CC([O-])=O.CC([O-])=O.[Pd+2]>[F:27][C:28]1[CH:33]=[CH:32][C:31](/[CH:34]=[CH:35]/[C:2]2[CH:7]=[CH:6][C:5]3[C:8]4[C:9]([NH:17][CH2:18][C:19]5[CH:20]=[CH:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=5)=[N:10][CH:11]=[C:12]([C:15]#[N:16])[C:13]=4[S:14][C:4]=3[CH:3]=2)=[CH:30][CH:29]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 5706776trans-2-(4-Fluorophenyl)vinylboronic acidHCID 591984657-Bromo-1-[(4-methoxybenzyl)amino][1]benzothieno[3,2-c]pyridine-4-carbonitrile

生成物 1

HCID 59198487HCID 59198487、化合物

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 10311-Propanol溶媒

反応条件

温度
100 °C

実験手順

To a suspension of 7-bromo-1-[(4-methoxybenzyl)amino][1]benzothieno[3,2-c]pyridine-4-carbonitrile (Example 12, Step 9) in 1-propanol (0.1 M) was added [(E)-2-(4-fluorophenyl)vinyl]boronic acid (1.5 equiv), 2.0 M aqueous Na2CO3 solution (2.5 equiv), and a 3:1 mixture of Ph3P:Pd(OAc)2 (0.1 equiv). The mixture was degassed and then stirred at 100° C. for 2.5 h, and was then partitioned between EtOAc/THF and H2O. The organic layer was washed with H2O and brine, and was then dried (MgSO4), filtered, and evaporated. The crude material was purified by flash chromatography, eluting with 1:1 Et2O:hexanes. The product was stirred with 1:10 EtOAc:hexanes containing trace acetone to yield the title compound as a pale yellow solid after filtration.

後処理

  1. customThe mixture was degassed
  2. customwas then partitioned between EtOAc/THF and H2O
  3. washThe organic layer was washed with H2O and brine
  4. dry with materialwas then dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude material was purified by flash chromatography
  8. washeluting with 1:1 Et2O
  9. stirringThe product was stirred with 1:10 EtOAc

出典と根拠

ORDレコード
ord-be1583acaf064d7aabe6385f22142d36
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08518964B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート