Water → 9-(2-acetoxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one

HRID 1681837ノート

反応式

HRID 1681837 の反応式
[OH:1][CH2:2][CH2:3][C:4]1[S:18][C:7]2[S:8][CH2:9][CH2:10][CH:11]3[CH2:16][C:15](=[O:17])[NH:14][N:13]=[C:12]3[C:6]=2[CH:5]=1.C(N(CC)CC)C.[C:26](OC(=O)C)(=[O:28])[CH3:27].O>C1(C)C=CC=CC=1>[C:26]([O:1][CH2:2][CH2:3][C:4]1[S:18][C:7]2[S:8][CH2:9][CH2:10][CH:11]3[CH2:16][C:15](=[O:17])[NH:14][N:13]=[C:12]3[C:6]=2[CH:5]=1)(=[O:28])[CH3:27]

参加物

6

反応物 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 190168139-(2-hydroxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one

生成物 1

HCID 190168369-(2-acetoxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 1.0 g of 9-(2-hydroxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one, 2 ml of triethylamine and 2 ml of acetic anhydride in 20 ml of toluene is kept on a water bath at 80°-85° C. for 3 hours. After cooling, to the mixture is added water, the organic layer is collected by a separatory funnel and concentrated. To the residue is added hexane and the precipitated crystals are collected by filtration. The resulting crystals are recrystallized from isopropyl ether to give 0.5 g of 9-(2-acetoxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one as white crystals, melting at 106°-108° C.

後処理

  1. temperatureAfter cooling, to the mixture
  2. customthe organic layer is collected by a separatory funnel
  3. concentrationconcentrated
  4. additionTo the residue is added hexane
  5. filtrationthe precipitated crystals are collected by filtration
  6. customThe resulting crystals are recrystallized from isopropyl ether

出典と根拠

ORDレコード
ord-e378d3ca9f7542fc9cf3e0c3735183dc
出典データセット
uspto-grants-1992_12
特許番号
US05175162

反応ノート

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