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Triphenylphosphine → (1-Benzenesulfonyl-1H-indol-5-yl)-[6-(3-imidazol-1-yl-prop-1-ynyl)-quinazolin-4-yl]-amine

HRID 1264050
ノート
印刷プレビュー

反応式

HRID 1264050 の反応式
[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][C:15]([NH:19][C:20]4[C:29]5[C:24](=[CH:25][CH:26]=[C:27](I)[CH:28]=5)[N:23]=[CH:22][N:21]=4)=[CH:16][CH:17]=3)[CH:12]=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:31]([N:34]1[CH:38]=[CH:37][N:36]=[CH:35]1)[C:32]#[CH:33].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>CCN(CC)CC.CN(C=O)C.CC([O-])=O.CC([O-])=O.[Pd+2]>[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][C:15]([NH:19][C:20]4[C:29]5[C:24](=[CH:25][CH:26]=[C:27]([C:33]#[C:32][CH2:31][N:34]6[CH:38]=[CH:37][N:36]=[CH:35]6)[CH:28]=5)[N:23]=[CH:22][N:21]=4)=[CH:16][CH:17]=3)[CH:12]=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=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 3

HCID 11776TriphenylphosphineHCID 125919421-(prop-2-yn-1-yl)-1H-imidazoleHCID 15450144(1-Benzenesulfonyl-1H-indol-5-yl)-(6-iodo-quinazolin-4-yl)-amine

生成物 1

HCID 18616501(1-Benzenesulfonyl-1H-indol-5-yl)-[6-(3-imidazol-1-yl-prop-1-ynyl)-quinazolin-4-yl]-amine収率 51%

試薬・触媒・溶媒 3

HCID 167845
palladium(II) acetate
触媒
HCID 6228Dimethylformamide溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
80 °C

実験手順

Quinazoline 14 (150 mg, 0.28 mmol), 1-N-2-propynylimidazole (200 mg, 1.89 mmol), Pd(OAc)2 (4 mg, 0.016 mmol) and PPh3 (9 mg, 0.033 mmol) were mixed in NEt3 (1.25 mL) and DMF (0.5 mL). The mixture was heated at 80° C under N2 for 16 hours. Upon cooling the black suspension was concentrated under reduced pressure and the residue dissolved in MeOH. Silica gel (1 g) was added and the methanol removed in vacuo. The resulting silica gel was placed atop a silica gel (40g) column which was then eluted with 200 mL 50:1 CH2Cl2:MeOH, the 300 mL 25:1 CH2Cl2 to provide alkyne 15 (72 mg, 51%) as a yellow foam. 1H NMR (CDCl3; 400 MHz): δ: 8.95 (br, 1H, NH), 8.63 (s, 1H), 8.62 (s, 1H), 8.24 (s, 1H), 7.96 (d, 1H, J=1.7 Hz), 7.84 (m, 3H), 7.71 (m, 2H), 7.51 (m, 3H), 7.41 (m, 2H), 7.14 (s, 1H), 7.10 (s, 1H), 6.55 (d, 1H, J=3.5 Hz), 5.01 (s, 2H).

後処理

  1. temperatureUpon cooling the black suspension
  2. concentrationwas concentrated under reduced pressure
  3. dissolutionthe residue dissolved in MeOH
  4. additionSilica gel (1 g) was added
  5. customthe methanol removed in vacuo
  6. washwas then eluted with 200 mL 50:1 CH2Cl2

出典と根拠

ORDレコード
ord-55ae7b210f0648e7913e32b905c97d43
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06541481B2

反応ノート

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