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Binap, (A+-)- → [3-(4-Benzyl-4,7-diaza-spiro[2.5]oct-7-yl)-isoquinolin-1-yl]-acetic acid ethyl ester

HRID 1767694
ノート
印刷プレビュー

反応式

HRID 1767694 の反応式
[CH2:1]([O:3][C:4](=[O:17])[CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]=[C:8](Cl)[N:7]=1)[CH3:2].[CH2:18]([N:25]1[CH2:32][CH2:31][NH:30][CH2:29][C:26]21[CH2:28][CH2:27]2)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.CC([O-])(C)C.[Na+].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:1]([O:3][C:4](=[O:17])[CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]=[C:8]([N:30]2[CH2:29][C:26]3([CH2:28][CH2:27]3)[N:25]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:32][CH2:31]2)[N:7]=1)[CH3:2]
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

6

反応物 4

HCID 634876Binap, (A+-)-HCID 11379685Ethyl 2-(3-chloroisoquinolin-1-yl)acetateHCID 113900664-Benzyl-4,7-diazaspiro[2.5]octaneHCID 23676156Sodium t-butoxide

生成物 1

HCID 11327484[3-(4-Benzyl-4,7-diaza-spiro[2.5]oct-7-yl)-isoquinolin-1-yl]-acetic acid ethyl ester

試薬・触媒・溶媒 1

HCID 167845
palladium(II) acetate
触媒

反応条件

温度
85 °C

実験手順

(3-Chloro-isoquinolin-1-yl)-acetic acid ethyl ester (2.50 g, 10.01 mmol), 4-benzyl-4,7-diaza-spiro [2.5]octane (2.23 g, 11.01 mmol), NaOtBu (1.06 g, 11.01 mmol), BINAP (249 mg, 0.40 mmol) and Palladium(II)-acetate (180 mg, 0.80 mmol) are mixed under argon. After addition of degassed, dry dioxane (36 ml), the suspension is heated to 85° C. After 25 minutes at 85° C., HPLC analysis indicates a conversion of 71%. The mixture is cooled to RT, diluted with EtOAc, and washed with H2O and sat. aq. NH4Cl (back extracted). The combined organic layers are dried over Na2SO4, the solvent is removed and the residue purified by FCC (hexane/EtOAc 100:0 to 96:4 to 93:7 to 90:10 to 85:15) to afford the title compound. 1H NMR (DMSO, 400 MHz) δ 0.58 -0.61 (m, 2H), 0.70 -0.73 (m, 2H), 1.18 (t, J=8.8, 3H), 2.98 (t, J =5.5, 2H), 3.39 (s, 2H), 3.49 (t, J=5.5, 2H), 3.86 (s, 2H), 4.12 (s, 2H), 4.12 (q, J=8.8, 2H), 5.59 (s, 1H), 7.14 -7.19 (m, 6H), 7.39 (t, J=8.8, 1H), 7.51 (d, J=9.9, 1H), 7.78 (d, J=9.9, 1H); ES-MS: 417 [M+H]+.

後処理

  1. additionAfter addition
  2. customof degassed
  3. temperatureThe mixture is cooled to RT
  4. additiondiluted with EtOAc
  5. washwashed with H2O and sat. aq. NH4Cl (back extracted)
  6. dry with materialThe combined organic layers are dried over Na2SO4
  7. customthe solvent is removed
  8. customthe residue purified by FCC (hexane/EtOAc 100:0 to 96:4 to 93:7 to 90:10 to 85:15)

出典と根拠

ORDレコード
ord-0cc93b0fbe184b91bf758bc8b3cc7289
出典データセット
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07235555B2

反応ノート

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