p-Toluenesulfonic acid → HCID 70655408、化合物

HRID 77340ノート

反応式

HRID 77340 の反応式
O[CH2:2][CH:3]1[CH2:7][O:6][C:5]2([CH2:12][CH2:11][N:10]([CH2:13][CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH2:9][CH2:8]2)[O:4]1.[C:21]1(C)[CH:26]=[CH:25][C:24]([S:27](O)(=O)=O)=[CH:23][CH:22]=1.C1(S)C=CC=CC=1>C1(C)C=CC=CC=1>[CH2:13]([N:10]1[CH2:9][CH2:8][C:5]2([O:4][CH:3]([CH2:2][S:27][C:24]3[CH:25]=[CH:26][CH:21]=[CH:22][CH:23]=3)[CH2:7][O:6]2)[CH2:12][CH2:11]1)[CH2:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

5

実験手順

2-hydroxymethyl-8-phenethyl-1,4-dioxa-8-azaspiro[4,5]decane (Compound 1, 50 gm, 0.18 mole) and Para Toluenesulfonic Acid (PTSA, 2 gm) were dissolved in toluene (350 ml) at room temperature. 20 gm of thiophenol was added drop wise to the above solution. The reaction was refluxed for 13 hrs at reflux temperature. The solvent was distilled off to get the light brown solid product with a melting point of 58° C. The yield of the product was 95%.

後処理

  1. temperatureThe reaction was refluxed for 13 hrs
  2. temperatureat reflux temperature
  3. distillationThe solvent was distilled off
  4. customto get the light brown solid product with a melting point of 58° C

出典と根拠

ORDレコード
ord-054d4a7a395e4bf7aa1e7ee4c889894b
出典データセット
uspto-grants-2014_09
特許番号
US08841296B2

反応ノート

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