ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Tri-o-tolylphosphine → HCID 16662046、化合物

HRID 2097012
ノート
印刷プレビュー

反応式

HRID 2097012 の反応式
[CH3:1][N:2]([CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][C:15]([F:18])([F:17])[F:16])[C:9]=1[O:19][CH2:20][CH2:21][CH3:22])[C:3](=[O:6])[CH:4]=[CH2:5].C(N(C(C)C)CC)(C)C.Br[C:33]1[CH:46]=[N:45][C:36]2[NH:37][C:38](=[O:44])[C:39]([CH3:43])([CH3:42])[NH:40][CH2:41][C:35]=2[CH:34]=1.CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C>C(#N)CC.CN(C=O)C.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH3:42][C:39]1([CH3:43])[C:38](=[O:44])[NH:37][C:36]2[N:45]=[CH:46][C:33](/[CH:5]=[CH:4]/[C:3]([N:2]([CH3:1])[CH2:7][C:8]3[CH:13]=[CH:12][CH:11]=[C:10]([O:14][C:15]([F:18])([F:16])[F:17])[C:9]=3[O:19][CH2:20][CH2:21][CH3:22])=[O:6])=[CH:34][C:35]=2[CH2:41][NH:40]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 80271Tri-o-tolylphosphineHCID 81531DiisopropylethylamineHCID 59277578N-Methyl-N-(2-propoxy-3-trifluoromethoxybenzyl)acrylamideHCID 594569147-Bromo-3,3-dimethyl-1,3,4,5-tetrahydropyrido[2,3-e][1,4]diazepin-2-one

生成物 1

HCID 16662046HCID 16662046、化合物収率 44.5%

試薬・触媒・溶媒 3

HCID 167845
palladium(II) acetate
触媒
HCID 6228Dimethylformamide溶媒
HCID 7854Propionitrile溶媒

実験手順

A solution of N-methyl-N-(2-propoxy-3-trifluoromethoxybenzyl)acrylamide (0.468 g, 1.47 mmol) in propionitrile (5 mL) and DMF (1 mL) was deoxygenated with Ar for 20 min. The solution was treated sequentially with diisopropylethylamine (0.40 mL, 2.3 mmol) and 7-bromo-3,3-dimethyl-1,3,4,5-tetrahydro-pyrido[2,3-e][1,4]diazepin-2-one (0.300 g, 1.11 mmol). The solution was deoxygenated with Ar for 20 min. Pd(OAc)2 (0.024 g, 0.111 mmol) and P(o-tol)3 (0.067 g, 0.222 mmol) were added and the solution was deoxygenated with Ar for 20 minutes. The mixture was heated to reflux for 18 h, then allowed to cool. The mixture was diluted with EtOAc (30 mL) and then washed with H2O (3×50 mL) and brine (2×100 mL), dried (Na2SO4) and concentrated to a yellow-orange solid. Purification by column chromatography (silica gel, CH2Cl2/MeOH, 100 to 98:2) gave the title compound (0.25 g, 31%) as an off-white solid and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-d6) δ 9.80-9.78 (m, 1H), 8.41-8.36 (m, 1H), 8.01-7.92 (m, 1H), 7.56-7.49 (m, 1H), 7.36-7.08 (m, 4H), 4.87-4.69 (m, 2H), 3.96-3.83 (m, 4H), 3.16-2.88 (m, 4H), 1.78-1.71 (m, 2H), 1.31-1.29 (m, 6H), 1.03-0.98 (m, 3H); MS (ESI) m/e 507 (M+H)+.

後処理

  1. customThe solution was deoxygenated with Ar for 20 min
  2. customthe solution was deoxygenated with Ar for 20 minutes
  3. temperatureThe mixture was heated
  4. temperatureto reflux for 18 h
  5. temperatureto cool
  6. additionThe mixture was diluted with EtOAc (30 mL)
  7. washwashed with H2O (3×50 mL) and brine (2×100 mL)
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated to a yellow-orange solid
  10. customPurification by column chromatography (silica gel, CH2Cl2/MeOH, 100 to 98:2)

出典と根拠

ORDレコード
ord-e80b96d803fc48849207bdb8edb54ad8
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450307B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート