Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 21024036、化合物

HRID 1795689ノート

反応式

HRID 1795689 の反応式
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.[Cl:18][CH2:19][C:20]([O:22][CH:23]1[C:24]([O:66]C(OCC)C)([CH3:65])[CH2:25][CH2:26][CH:27]([O:59]C(OCC)C)[CH2:28][C:29]([O:31][CH:32](/[C:37](/[CH3:58])=[CH:38]/[CH:39]=[CH:40]/[CH:41]([CH3:57])[CH2:42][CH:43]2[O:56][CH:44]2[CH:45]([CH3:55])[CH:46]([O:49]C(OCC)C)[CH2:47][CH3:48])[CH:33]([CH3:36])[CH:34]=[CH:35]1)=[O:30])=[O:21]>CO>[Cl:18][CH2:19][C:20]([O:22][CH:23]1[C:24]([OH:66])([CH3:65])[CH2:25][CH2:26][CH:27]([OH:59])[CH2:28][C:29]([O:31][CH:32](/[C:37](/[CH3:58])=[CH:38]/[CH:39]=[CH:40]/[CH:41]([CH3:57])[CH2:42][CH:43]2[O:56][CH:44]2[CH:45]([CH3:55])[CH:46]([OH:49])[CH2:47][CH3:48])[CH:33]([CH3:36])[CH:34]=[CH:35]1)=[O:30])=[O:21]

参加物

4

反応物 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 21024035HCID 21024035、化合物

生成物 1

HCID 21024036HCID 21024036、化合物収率 70%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Pyridinium p-toluenesulfonate (1 mg, 4.1 μmol) was added to a solution of (8E,12E,14E)-7-chloroacetoxy-3,6,21-tri(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide (3.2 mg, 4.06 μmol) in methanol (1 mL), followed by stirring at room temperature for one hour. The reaction solution was evaporated, and the resulting residue was purified by thin layer chromatography (MERCK Silica gel 60 F254, 0.2 mm, developing solution; ethyl acetate-hexane=2:1) to obtain the title compound (1.6 mg, 70%) as a colorless oil.

後処理

  1. customThe reaction solution was evaporated
  2. customthe resulting residue was purified by thin layer chromatography (MERCK Silica gel 60 F254, 0.2 mm, developing solution; ethyl acetate-hexane=2:1)

出典と根拠

ORDレコード
ord-b1893cbd9d8e4068a07772c5bcf37a48
出典データセット
uspto-grants-2006_04
特許番号
US07026352B1

反応ノート

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