Oxygen → HCID 178481257、化合物

HRID 2240640ノート

反応式

HRID 2240640 の反応式
C(OC(=O)[NH:6][C:7]1([C:10]2[CH:15]=[CH:14][C:13]([C:16]([NH:27][C:28]3[CH:33]=[CH:32][C:31]([C:34]4[N:35]=[CH:36][N:37]([CH3:39])[CH:38]=4)=[CH:30][CH:29]=3)=[C:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[O:19][C:18]3=[O:26])=[CH:12][CH:11]=2)[CH2:9][CH2:8]1)C=C.O=O.C(NCC)C>ClCCl.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>[NH2:6][C:7]1([C:10]2[CH:15]=[CH:14][C:13]([C:16]([NH:27][C:28]3[CH:33]=[CH:32][C:31]([C:34]4[N:35]=[CH:36][N:37]([CH3:39])[CH:38]=4)=[CH:30][CH:29]=3)=[C:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[O:19][C:18]3=[O:26])=[CH:12][CH:11]=2)[CH2:8][CH2:9]1

参加物

6

反応物 3

HCID 977OxygenHCID 8021DiethylamineHCID 178459817HCID 178459817、化合物

生成物 1

HCID 178481257HCID 178481257、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

0.58 g of allyl(1-{4-[[4-(1-methyl-1H-imidazol-4-yl)phenylamino]-(2-oxobenzofuran-3-ylidene)methyl]phenyl}cyclopropyl)carbamate was dissolved in 20 mL of dichloromethane. The solution was freed from oxygen using argon. Then at RT, 0.52 mL of diethylamine and 0.058 g of tetrakis(triphenylphosphine)palladium (0) were added. The mixture was stirred for 2 hours at RT, the suspension was evaporated down with silica gel and chromatographed with dichloromethane/methanol (97:3) on silica gel 70 at a flow rate of 30 mL/min. The clean fractions were combined, evaporated down to the residue, dissolved in dichloromethane, filtered, and combined with diisopropyl ether. The dichloromethane was distilled off, the crystals formed were suction filtered and washed with diisopropyl ether. Yield: 0.26 g of yellow crystals, melting point 190° C.-191° C., as base. Rf value: 0.51 (dichloromethane/methanol (9:1)).

後処理

  1. customthe suspension was evaporated down with silica gel
  2. customchromatographed with dichloromethane/methanol (97:3) on silica gel 70 at a flow rate of 30 mL/min
  3. customevaporated down to the residue
  4. dissolutiondissolved in dichloromethane
  5. filtrationfiltered
  6. distillationThe dichloromethane was distilled off
  7. customthe crystals formed
  8. filtrationwere suction filtered
  9. washwashed with diisopropyl ether

出典と根拠

ORDレコード
ord-a598db9684da4d2b94d8573f8818fe8c
出典データセット
uspto-grants-2010_05
特許番号
US07723381B2

反応ノート

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