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Ethyl 2-(tributylstannyl)acetate → Ethyl 2-(3-(benzyloxy)naphthalen-1-yl)acetate

HRID 900149
ノート
印刷プレビュー

反応式

HRID 900149 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11](Br)[C:12]2[C:17]([CH:18]=1)=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:20]([O:22][C:23](=[O:38])[CH2:24][Sn](CCCC)(CCCC)CCCC)[CH3:21]>CN(C=O)C.CCOC(C)=O.[Br-].[Zn+2].[Br-]>[CH2:20]([O:22][C:23](=[O:38])[CH2:24][C:11]1[C:12]2[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:18]=[C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:10]=1)[CH3:21]
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 2

HCID 10894129Ethyl 2-(tributylstannyl)acetateHCID 211145093-(Benzyloxy)-1-bromonaphthalene

生成物 1

HCID 44479435Ethyl 2-(3-(benzyloxy)naphthalen-1-yl)acetate

試薬・触媒・溶媒 3

HCID 10421208Zinc bromide触媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate
溶媒

反応条件

温度
80 °C

実験手順

3-Benzyloxy-1-bromo-naphthalene (5.64 g, 18.01 mmol) is dissolved under an atmosphere of argon in dry DMF (100 ml). Tributylstannanyl-acetic acid ethyl ester (7.47 g, 19.81 mmol) is added, as well as [bis(tri-ortho-tolyl-phosphine)]palladium (II) dichloride (2.83 g, 3.60 mmol) and zinc(II) bromide (5.27 g, 23.41 mmol). The reaction mixture is heated to 80° C. for 3 h. The reaction mixture is diluted with EtOAc and washed twice with diluted brine (back extracted). The combined organic layers are dried over Na2SO4, the solvent is removed, and the residue is purified by FCC (hexane/EtOAc 100:0 to 97.5:2.5 to 95:5 to 90:10). The resulting oil, still containing tin residues, is stirred in a 1:1 mixture of EtOAc/1N NaOH (200 ml) for 1 h. The mixture is extracted twice with EtOAc. The combined organic layers are washed twice with H2O (back extracted), dried over Na2SO4 and concentrated. The residue is purified by FCC (hexane/EtOAc 100:0 to 97:3 to 95:5 to 93:7 to 92:8 to 90:10) to yield the title compound. 1H NMR (DMSO, 400 MHz) δ 1.18 (t, J=7.2 Hz, 3H), 4.10 (q, J=7.2 Hz, 2H), 4.11 (s, 2H), 5.25 (s, 2H), 7.21 (d, J=3.0 Hz, 1H), 7.41 (m, 8H), 7.53 (d, J=6.6 Hz, 1H), 7.84 (dd, J=7.2 Hz, 1H); ES-MS: 320 [M+H]+.

後処理

  1. washwashed twice with diluted brine (back extracted)
  2. dry with materialThe combined organic layers are dried over Na2SO4
  3. customthe solvent is removed
  4. customthe residue is purified by FCC (hexane/EtOAc 100:0 to 97.5:2.5 to 95:5 to 90:10)
  5. extractionThe mixture is extracted twice with EtOAc
  6. washThe combined organic layers are washed twice with H2O (back extracted)
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated
  9. customThe residue is purified by FCC (hexane/EtOAc 100:0 to 97:3 to 95:5 to 93:7 to 92:8 to 90:10)

出典と根拠

ORDレコード
ord-c3a78a795fe043a886bdcfb63f4d5869
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07358253B2

反応ノート

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