Water → HCID 10458258、化合物

HRID 898920ノート

反応式

HRID 898920 の反応式
[C:1]([C:5]1[CH:37]=[CH:36][C:8]([CH2:9][N:10]([CH2:34][CH3:35])[C:11](=[O:33])[CH2:12][O:13][C:14]2[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][O:22][C:23]3[CH:32]=[CH:31][CH:30]=[CH:29][C:24]=3[C:25]([O:27]C)=[O:26])=[CH:16][CH:15]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].O>C1COCC1>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][N:10]([CH2:34][CH3:35])[C:11](=[O:33])[CH2:12][O:13][C:14]2[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][O:22][C:23]3[CH:32]=[CH:31][CH:30]=[CH:29][C:24]=3[C:25]([OH:27])=[O:26])=[CH:16][CH:15]=2)=[CH:36][CH:37]=1)([CH3:3])([CH3:2])[CH3:4]

参加物

4

反応物 2

HCID 962WaterHCID 69259345HCID 69259345、化合物

生成物 1

HCID 10458258HCID 10458258、化合物収率 73.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 2-[2-(4-{2-[(4-tert-butylbenzyl)(ethyl)amino]-2-oxoethoxy}phenyl)-ethoxy]benzoate (0.2290 g, 0.455 mmol) was dissolved in a mixture of THF (freshly distilled)/water (2/1, 3 ml), lithium-hydroxide (0.218 g, 0.909 mmol) was added. The reaction was performed in a single node microwave oven (5 min, 150 deg). THF was removed by evaporation. Water was added (10 ml) and the basic water phase was washed with diethyl ether (2×10 ml). Addition of HCl (2 ml, 1 M, pH 1). The water phase was extracted with two portions of DCM (20 ml), the organic phase was dried (MgSO4) and the solvent was removed by evaporation to give 0.163 g of 2-[2-(4-{2-[(4-tert-butylbenzyl)(ethyl)amino]-2-oxoethoxy}phenyl)ethoxy]benzoic acid (yield 73.2%).

後処理

  1. additionwas added
  2. customThe reaction was performed in a single node microwave oven
  3. custom(5 min, 150 deg)
  4. customTHF was removed by evaporation
  5. additionWater was added (10 ml)
  6. washthe basic water phase was washed with diethyl ether (2×10 ml)
  7. additionAddition of HCl (2 ml, 1 M, pH 1)
  8. extractionThe water phase was extracted with two portions of DCM (20 ml)
  9. dry with materialthe organic phase was dried (MgSO4)
  10. customthe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-ade79e29917b483dbdea461d06e18387
出典データセット
uspto-grants-2008_04
特許番号
US07351858B2

反応ノート

読み込み中…