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HCID 68485937、化合物 → HCID 68485225、化合物

HRID 1874903
ノート
印刷プレビュー

反応式

HRID 1874903 の反応式
[NH2:1][CH2:2][C:3]1[C:4]([F:20])=[C:5]([O:10][C:11]2[CH:12]=[C:13]([CH:16]=[C:17](Br)[CH:18]=2)[C:14]#[N:15])[C:6]([Cl:9])=[CH:7][CH:8]=1.[CH2:21]([Zn]CC)[CH3:22]>C1COCC1.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>[NH2:1][CH2:2][C:3]1[C:4]([F:20])=[C:5]([O:10][C:11]2[CH:12]=[C:13]([CH:16]=[C:17]([CH2:21][CH3:22])[CH:18]=2)[C:14]#[N:15])[C:6]([Cl:9])=[CH:7][CH:8]=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

5

反応物 2

HCID 68485937HCID 68485937、化合物HCID 178418750HCID 178418750、化合物

生成物 1

HCID 68485225HCID 68485225、化合物収率 62.1%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

3-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-bromobenzonitrile (0.400 g, 1.125 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.130 g, 0.112 mmol) were combined in THF (7 mL) and treated with diethylzinc (1 M in heptane) (2.250 mL, 2.250 mmol) with stirring under an inert atmosphere. The reaction mixture was heated to 70° C. and stirred for 2 h. The reaction mixture was concentrated to dryness and partitioned between EtOAc and saturated aqueous NaHCO3. The organic phase was isolated, dried over MgSO4, filtered and concentrated to dryness. The residue was purified on 40 g silica gel eluted successively with EtOAc and 10% CH3OH/DCM to give 3-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-ethylbenzonitrile (0.213 g, 0.699 mmol, 62.1% yield) as a clear oil. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.44-7.54 (m, 3H), 7.12-7.20 (m, 2H), 3.76 (s, 2H), 2.64 (q, J=7.60 Hz, 2H), 1.90 (br. s., 2H), 1.15 (t, J=7.55 Hz, 3H). LC-MS (ES−) m/z 303.25, 305.16 [M−1]. LC-MS (ES+) m/z 305.01, 306.98 [M+H].

後処理

  1. stirringstirred for 2 h
  2. concentrationThe reaction mixture was concentrated to dryness
  3. custompartitioned between EtOAc and saturated aqueous NaHCO3
  4. customThe organic phase was isolated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated to dryness
  8. customThe residue was purified on 40 g silica gel
  9. washeluted successively with EtOAc and 10% CH3OH/DCM

出典と根拠

ORDレコード
ord-499ad5c78fa041e3b018e84baed0320a
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08304419B2

反応ノート

読み込み中…

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