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

HRID 1728935노트

반응식

HRID 1728935 반응식
[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]

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-009ea3f0ffe34381bec1ae75920209c7
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05329016

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