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Sodium Iodide → (R)-3-iodo-1-phenyl-1-propanol

HRID 269998
ノート
印刷プレビュー

反応式

HRID 269998 の反応式
[I-:1].[Na+].Cl[CH2:4][CH2:5][C@H:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[OH:7]>CC(C)=O>[I:1][CH2:4][CH2:5][C@H:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[OH:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 642409(1R)-3-chloro-1-phenylpropan-1-ol

生成物 1

HCID 14476875(R)-3-iodo-1-phenyl-1-propanol収率 92.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Add sodium iodide (4.29 g, 29 mmol) to a solution of (R)-(+)-3-chloro-1-phenyl-1-propanol (0.5 g, 2.93 mmol) in acetone (9.75 mL), and heat to reflux overnight. Cool and filter the suspension, then remove the volatiles under reduced pressure. Resuspend the residue in ether, filter and evaporate to afford (R)-3-iodo-1-phenyl-1-propanol (0.71 g). Add (R)-3-iodo-1-phenyl-1-propanol (0.1 g, 0.4 mmol) to a solution of 7-phenyl-isoquinoline -5-sulfonic acid (2-amino-ethyl)-amide (0.087 g, 0.27 mmol) in DMF (0.5 mL) and DCE (0.27 mL) containing diisopropylethylamine (0.094 mL, 0.53 mmol), and warm to 80° C. for 30 minutes. Cool to ambient temperature, and apply to a cation exchange resin cartridge. Wash with methanol, and elute product from the resin with 2M methanolic ammonia. Evaporate and purify the residue by silica gel chromatography using a methanol-methylene chloride gradient, followed by treatment with aqueous hydrochloric acid and lyophylization to afford the title compound. 1H NMR (DMSO): δ9.71(s, 1H), 9.00-8.82 (m, 3H), 8.80-8.73(m, 2H), 8.69 (d, J=1.8 Hz, 1H), 8.59 (d, J=6.2 Hz, 1H), 7.95 (dd, J1=1.5 Hz, J2=8.5 Hz, 2H), 7.62 (t, J=6.7 Hz, 2H), 7.53 (t, J=7.8 Hz, 1H), 7.38-7.29 (m, 4H), 7.28-7.21 (m, 1H), 5.50-4.67 (bs, 2H), 4.65 (dd, J1=4.5 Hz, J2=8.5 Hz, 1H), 3.23-3.10 (m, 2H), 3.06-2.86 (m, 4H), 2.00=−1.77(m, 2H). LCMS: m/z 462(M+H)+460(M−H)−.

後処理

  1. temperatureheat
  2. temperatureto reflux overnight
  3. temperatureCool
  4. filtrationfilter the suspension
  5. customremove the volatiles under reduced pressure
  6. filtrationfilter
  7. customevaporate

出典と根拠

ORDレコード
ord-0114795f954b4f16a2b6ba2ce3aafcde
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07449477B2

反応ノート

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