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2-Methoxyethylamine → [2-(4-Isopropyl-4H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulen-8-ylmethyl]-(2-methoxy-ethyl)-amine

HRID 2385665
ノート
印刷プレビュー

反応式

HRID 2385665 の反応式
[CH:1]([N:4]1[CH:8]=[N:7][N:6]=[C:5]1[C:9]1[S:10][C:11]2[CH2:12][CH2:13][O:14][C:15]3[CH:22]=[C:21]([CH:23]=O)[CH:20]=[CH:19][C:16]=3[C:17]=2[N:18]=1)([CH3:3])[CH3:2].[CH3:25][O:26][CH2:27][CH2:28][NH2:29]>>[CH:1]([N:4]1[CH:8]=[N:7][N:6]=[C:5]1[C:9]1[S:10][C:11]2[CH2:12][CH2:13][O:14][C:15]3[CH:22]=[C:21]([CH2:23][NH:29][CH2:28][CH2:27][O:26][CH3:25])[CH:20]=[CH:19][C:16]=3[C:17]=2[N:18]=1)([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 80182-MethoxyethylamineHCID 582037272-(4-Isopropyl-4H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-8-carbaldehyde

生成物 1

HCID 58204241[2-(4-Isopropyl-4H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulen-8-ylmethyl]-(2-methoxy-ethyl)-amine収率 56%

実験手順

Following the procedure for 119, 2-(4-isopropyl-4H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-8-carbaldehyde and 2-methoxyethylamine were reacted. After purification by flash chromatography the resulting oil was dissolved in ether and treated with 1M HCl in ether to give a solid that was filtered off and dried to give 120 as a yellow solid (129 mg, 56%). LCMS: RT=6.11 min, [M+H]+=400. 1H NMR δ (ppm) (DMSO-d6): 9.17 (2 H, s), 8.93-8.90 (1 H, m), 8.29 (1 H, d, J=8.13 Hz), 7.28 (1 H, dd, J=8.22, 1.81 Hz), 7.24 (1 H, d, J=1.76 Hz), 5.47-5.38 (1 H, m), 4.33 (2 H, t, J=4.98 Hz), 4.10 (2 H, t, J=5.38 Hz), 3.56 (2 H, t, J=5.15 Hz), 3.43-3.30 (2 H, m), 3.25 (3 H, s), 3.02 (2 H, t, J=5.63 Hz), 1.56-1.49 (6 H, m)

後処理

  1. customwere reacted
  2. customAfter purification by flash chromatography the resulting oil
  3. dissolutionwas dissolved in ether
  4. additiontreated with 1M HCl in ether
  5. customto give a solid
  6. filtrationthat was filtered off
  7. customdried

出典と根拠

ORDレコード
ord-714aba6c90e842938fbef00d2233a865
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263633B2

反応ノート

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