Water → HCID 69199600、化合物

HRID 2252237ノート

反応式

HRID 2252237 の反応式
[CH:1](OCC)=[O:2].[H-].[Na+].[CH3:8][O:9][C:10]1[CH:18]=[C:17]2[C:13]([CH2:14][CH2:15][C:16]2=[O:19])=[CH:12][CH:11]=1.O>C1C=CC=CC=1>[OH:2][CH:1]=[C:15]1[CH2:14][C:13]2[C:17](=[CH:18][C:10]([O:9][CH3:8])=[CH:11][CH:12]=2)[C:16]1=[O:19]

参加物

6

反応物 4

HCID 962WaterHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 3340366-Methoxy-1-Indanone

生成物 1

HCID 69199600HCID 69199600、化合物収率 91%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To a mixture of ethyl formate (15.75 mL, 0.195 mol) and NaH (60%, 7.80 g, 0.195 mol) in benzene (550 mL) was added a suspension of 6-methoxy-indan-1-one (15.81 g, 0.0974 mol) in benzene (150 mL) dropwise at 0° C. The reaction mixture was stirred at room temperature overnight and treated with water. The solid was filtered, washed with water, and oven dried to give the desired product (16.86 g, 91%). The product may exist in sodium salt form, however, it was carried into the next reaction without further characterization. MS (DCI/NH3) m/z: 191.1 (M+H)+; 1H NMR (300 MHz, DMSO-D6) δ ppm 3.50 (s, 2H) 3.80 (s, 3H) 7.13-7.20 (m, 2H) 7.47 (d, J=8.14 Hz, 1H) 7.74 (s, brd, 1H).

後処理

  1. additionwas added
  2. filtrationThe solid was filtered
  3. washwashed with water, and oven
  4. customdried

出典と根拠

ORDレコード
ord-f92fa25e67e74244afe60b5de043f96f
出典データセット
uspto-grants-2008_01
特許番号
US07320986B2

反応ノート

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