Dichloromethane → HCID 86668414、化合物

HRID 2404098ノート

反応式

HRID 2404098 の反応式
[CH2:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[CH2:5][CH2:4][CH:3]([O:12][C:13]2[CH:14]=[C:15]3[C:20](=[CH:21][CH:22]=2)[CH:19]=[C:18]([CH2:23][OH:24])[CH:17]=[CH:16]3)[CH2:2]1.C(Cl)Cl.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>>[CH2:5]1[C:6]2([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]2)[CH2:1][CH2:2][CH:3]([O:12][C:13]2[CH:14]=[C:15]3[C:20](=[CH:21][CH:22]=2)[CH:19]=[C:18]([CH:23]=[O:24])[CH:17]=[CH:16]3)[CH2:4]1

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 159087TriacetoxyperiodinaneHCID 66926446(6-(Spiro[5.5]undecan-3-yloxy)naphthalen-2-yl)methanol

生成物 1

HCID 86668414HCID 86668414、化合物

実験手順

To [6-(Spiro[5.5]undec-3-yloxy)-naphthalen-2-yl]-methanol (150 mg, 0.46 mmol) in methylene chloride (5 mL, 80 mmol) was added Dess-Martin periodinane (0.274 g, 0.647 mmol) and the resulting solution was stirred at room temperature for 1 hour. The crude reaction was then passed through a silica gel plug, the filtrate was removed under vacuum to give 6-(spiro[5.5]undecan-3-yloxy)-2-naphthaldehyde as a colorless solid. (0.150 g, 100%). 1H NMR (400 MHz, CDCl3) δ 10.09 (s, 1H), 8.25 (s, 1H), 7.92-7.89 (m, 2H), 7.78 (d, J=8.7 Hz, 1H), 7.24-7.19 (m, 2H), 4.48 (m, 1H), 1.96-1.29 (m, 18H).

後処理

  1. customThe crude reaction
  2. customthe filtrate was removed under vacuum

出典と根拠

ORDレコード
ord-f7fa6e7bba7f40ba97876ed501ed19bb
出典データセット
uspto-grants-2014_08
特許番号
US08802659B2

反応ノート

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