p-Anisoyl chloride → HCID 9886338、化合物

HRID 2288585ノート

反応式

HRID 2288585 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:13]3[S:14][CH:15]=[CH:16][C:12]=3[CH2:11][CH2:10][NH:9]2)=[CH:4][CH:3]=1.[CH3:17][O:18][C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[C:13]3[S:14][CH:15]=[CH:16][C:12]=3[CH2:11][CH2:10][N:9]2[C:23]([C:22]2[CH:26]=[CH:27][C:19]([O:18][CH3:17])=[CH:20][CH:21]=2)=[O:24])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 7477p-Anisoyl chlorideHCID 8471TriethylamineHCID 186996347-(4-Chlorophenyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridine

生成物 1

HCID 9886338HCID 9886338、化合物収率 91%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

7-(4-Chloro-phenyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridin (100 mg) in toluene (20 ml), 4-methoxybenzoyl chloride (68.3 mg) and triethylamine (1 ml) were mixed and the mixture stirred at RT for 2 h. The reaction mixture was extracted once with NaOH (1 M) and once with water, the organic phase dried (MgSO4) and evaporated to dryness resulting in yellow oil which was purified on silica gel using methylene chloride/methanol 19/1 as eluent. The resulting oil was treated with abs ethanol resulting in precipitation of crystals. Yield 91%, m.p. 129.5-130.0 C. MS. M+=383.

後処理

  1. extractionThe reaction mixture was extracted once with NaOH (1 M) and once with water
  2. dry with materialthe organic phase dried (MgSO4)
  3. customevaporated to dryness
  4. customresulting in yellow oil which
  5. customwas purified on silica gel
  6. additionThe resulting oil was treated with abs ethanol resulting in precipitation of crystals

出典と根拠

ORDレコード
ord-ef0b3deb5c2c417e812c25ff873d8406
出典データセット
uspto-grants-2000_07
特許番号
US06090797

反応ノート

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