Lithium hydroxide, monohydrate → HCID 6102685、化合物

HRID 631872ノート

反応式

HRID 631872 の反応式
C[O:2][C:3]([C:5]1[C:14]2[CH2:13][CH2:12][CH2:11][CH2:10][C:9]=2[CH:8]=[CH:7][C:6]=1[NH:15][S:16]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:18])=[O:17])=[O:4].O.[OH-].[Li+]>O1CCOCC1.O.Cl>[C:19]1([S:16]([NH:15][C:6]2[CH:7]=[CH:8][C:9]3[CH2:10][CH2:11][CH2:12][CH2:13][C:14]=3[C:5]=2[C:3]([OH:4])=[O:2])(=[O:18])=[O:17])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

参加物

6

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 68296414HCID 68296414、化合物2 回

生成物 1

HCID 6102685HCID 6102685、化合物

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
160 °C

実験手順

2-Benzenesulfonylamino-5,6,7,8-tetrahydronaphthalene-1-carboxylic acid methyl ester (Intermediate 4, 0.68 g) was dissolved in dioxane (12 mL) and a solution of lithium hydroxide monohydrate (0.6 g) in water (6 mL) was added. The mixture was heated by microwave irradiation at 160° C. for 15 minutes then diluted with 1N hydrochloric acid. The product was extracted into DCM and the organic solution was separated, dried with magnesium sulfate, filtered and the filtrate was concentrated under vacuum to give the title compound as a white powder.

後処理

  1. extractionThe product was extracted into DCM
  2. customthe organic solution was separated
  3. dry with materialdried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated under vacuum

出典と根拠

ORDレコード
ord-fa8d3775e09b43e495bea60c20e989b5
出典データセット
uspto-grants-2016_04
特許番号
US09321740B2

反応ノート

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