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Phenol → (R)-tert-butyl (3-hydroxy-3-(3-(pyridin-4-ylmethoxy)phenyl)propyl)carbamate

HRID 2277045
ノート
印刷プレビュー

反応式

HRID 2277045 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+].C1(O)C=CC=CC=1.[OH:22][C@@H:23]([C:34]1[CH:39]=[CH:38][CH:37]=[C:36]([OH:40])[CH:35]=1)[CH2:24][CH2:25][NH:26][C:27](=[O:33])[O:28][C:29]([CH3:32])([CH3:31])[CH3:30]>CC(C)=O.CCOC(C)=O.O>[OH:22][C@@H:23]([C:34]1[CH:39]=[CH:38][CH:37]=[C:36]([O:40][CH2:2][C:3]2[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=2)[CH:35]=1)[CH2:24][CH2:25][NH:26][C:27](=[O:33])[O:28][C:29]([CH3:32])([CH3:31])[CH3:30]
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 996PhenolHCID 11430Potassium CarbonateHCID 6427994-(Bromomethyl)pyridineHCID 90405310(R)-tert-butyl 3-hydroxy-3-(3-hydroxyphenyl)propylcarbamate

生成物 1

HCID 90444193(R)-tert-butyl (3-hydroxy-3-(3-(pyridin-4-ylmethoxy)phenyl)propyl)carbamate

試薬・触媒・溶媒 3

HCID 180
Acetone
溶媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

4-(Bromomethyl)pyridine (298 mg, 1.17 mmol) and K2CO3 (774 mg, 5.61 mmol) were added to a solution of phenol (7, Intermediate I) (300 mg, 1.12 mmol) in acetone (20 mL). The reaction mixture was stirred overnight at ambient temperature, diluted with EtOAc and water. The organic layer was washed with 5% aq. NaOH, dried over anhydrous Na2SO4 and concentrated under reduced pressure. Purification by flash chromatography (50% EtOAc:hexane) gave (R)-tert-butyl (3-hydroxy-3-(3-(pyridin-4-ylmethoxy)phenyl)propyl)carbamate (15) as dark brown solid. Yield (0.183 g, 46%); 1H NMR (400 MHz, DMSO-d6): δ 8.61 (d, J=5.2 Hz, 2H), 7.36 (d, J=5.2 Hz, 2H), 7.28-7.24 (m, 1H), 7.03 (s, 1H), 6.96 (d, J=8.0 Hz, 1H), 6.85-6.83 (m, 1H), 5.10 (s, 2H), 4.86 (bs, 1H), 4.74-4.71 (m, 1H), 3.52-3.49 (m, 1H), 3.39 (bs, 1H), 3.19-3.12 (m, 1H), 1.86-1.77 (m, 2H), 1.45 (s, 9H); MS: m/z 359.19 [M+H]+.

後処理

  1. washThe organic layer was washed with 5% aq. NaOH
  2. dry with materialdried over anhydrous Na2SO4
  3. concentrationconcentrated under reduced pressure
  4. customPurification by flash chromatography (50% EtOAc:hexane)

出典と根拠

ORDレコード
ord-5f61ca2ffa284be2ae3d72df76ceea38
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133154B2

反応ノート

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