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4-Formylphenyl 4-(heptyloxy)benzoate → 4-(((2-(Tert-butoxy)-2-oxoethyl)amino)methyl)phenyl 4-(heptyloxy)benzoate

HRID 923552
ノート
印刷プレビュー

反応式

HRID 923552 の反応式
[CH2:1]([O:8][C:9]1[CH:25]=[CH:24][C:12]([C:13]([O:15][C:16]2[CH:21]=[CH:20][C:19]([CH:22]=O)=[CH:18][CH:17]=2)=[O:14])=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].Cl.[NH2:27][CH2:28][C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C1COCC1.C([O-])(O)=O.[Na+]>[CH2:1]([O:8][C:9]1[CH:25]=[CH:24][C:12]([C:13]([O:15][C:16]2[CH:21]=[CH:20][C:19]([CH2:22][NH:27][CH2:28][C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])=[CH:18][CH:17]=2)=[O:14])=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 17122224-Formylphenyl 4-(heptyloxy)benzoateHCID 2725036Glycine tert-butyl ester hydrochlorideHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 892531264-(((2-(Tert-butoxy)-2-oxoethyl)amino)methyl)phenyl 4-(heptyloxy)benzoate収率 19%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒
HCID 516892
Sodium Bicarbonate
溶媒

実験手順

Prepared using General Procedure 12: To a stirring solution of 4-formylphenyl 4-(heptyloxy)benzoate INT-12 (6.0 g, 17.6 mmol) in THF (30 mL) was added tert-butyl 2-aminoacetate hydrochloride (3.3 g, 19.7 mmol). After stirring for 2 h, sodium triacetoxyborohydride (7.5 g, 32.3 mmol) was added. After stirring for 12 h, the reaction mixture was diluted with NaHCO3 and the organic layer was separated. The remaining aqueous layer was extracted with DCM. The organic layers were combined, dried over Na2SO4, concentrated and purified by chromatography (EA/hexanes) to afford 155 mg (19%) of 4-(((2-(tert-butoxy)-2-oxoethyl)amino)methyl)phenyl 4-(heptyloxy)benzoate INT-13. LCMS-ESI (m/z) calculated for C27H37NO5: 455; found 456 [M+H]+, tR=3.27 min (Method 1). 1H NMR (400 MHz, CDCl3) δ 8.18-8.09 (m, 2H), 7.41 (d, J=8.5 Hz, 2H), 7.18-7.08 (m, 2H), 7.01-6.88 (m, 2H), 4.08-3.98 (m, 2H), 3.78 (s, 2H), 3.23 (s, 2H), 1.89-1.75 (m, 2H), 1.55-1.41 (s, 9H), 1.45-1.21 (m, 6H), 1.15-1.06 (m, 2H), 0.88 (dd, J=8.5, 5.0 Hz, 3H).

後処理

  1. customPrepared
  2. stirringAfter stirring for 12 h
  3. customthe organic layer was separated
  4. extractionThe remaining aqueous layer was extracted with DCM
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. custompurified by chromatography (EA/hexanes)

出典と根拠

ORDレコード
ord-9d7da54ba12e44a7b6928f25bce8ca90
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278910B2

反応ノート

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