Water → HCID 70533310、化合物

HRID 435449ノート

反応式

HRID 435449 の反応式
[C:1]1([C:7]2[C:8]3[O:13][CH2:12][O:11][CH:10](O)[C:9]=3[CH:15]=[CH:16][C:17]=2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=S(Cl)[Cl:26].C(Cl)Cl.O>CCOCC.N1C=CC=CC=1>[C:1]1([C:7]2[C:8]3[O:13][CH2:12][O:11][CH:10]([Cl:26])[C:9]=3[CH:15]=[CH:16][C:17]=2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

7

反応物 4

HCID 962WaterHCID 6344DichloromethaneHCID 24386Thionyl ChlorideHCID 70532672HCID 70532672、化合物

生成物 1

HCID 70533310HCID 70533310、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 3283Diethyl Ether溶媒2 回

実験手順

To a stirred solution of 11.6 g. (38 mmol) of 3,4-diphenylmethylenedioxybenzyl alcohol in ether (80 ml.) and pyridine (0.6 ml.) at 20° C. was added dropwise a solution of SOCl2 in ether (40 ml.). The mixture was cooled to 0°-5° C., and CH2Cl2 and water were added. The layers were separated, and the organic layer was washed with water and saturated aqueous NaCl, dried over MgSO4 and concentrated to dryness to yield 3,4-diphenylmethylenedioxybenzyl chloride (11.43 g.) as a colorless viscous oil: tlc (silica gel CH2Cl2 : Rf 0.8; ir (CCl4) no --OH--, nmr (CCl4) δ 4.34 (s, 2H), 6.74 (d,j=8) 2H, 6.67 (s, 1H), 7.1-7.6 (m, 10H). ##STR11##

後処理

  1. temperatureThe mixture was cooled to 0°-5° C.
  2. customThe layers were separated
  3. washthe organic layer was washed with water and saturated aqueous NaCl
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-184d5f6240034e1bb527e37469b92536
出典データセット
uspto-grants-1983_08
特許番号
US04401676

反応ノート

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