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Hydrochloric Acid → HCID 178442243、化合物

HRID 216408
ノート
印刷プレビュー

反応式

HRID 216408 の反応式
Cl.[CH3:2][C:3]([CH3:37])([CH3:36])[CH2:4][C:5]1[N:6]=[C:7]([CH:16]([OH:35])[C:17]2([C:23]3[CH:28]=[CH:27][C:26]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=4)=[CH:25][CH:24]=3)[S:22][CH2:21][CH2:20][CH2:19][S:18]2)[N:8](S(N(C)C)(=O)=O)[CH:9]=1>O1CCCC1>[CH3:2][C:3]([CH3:37])([CH3:36])[CH2:4][C:5]1[N:6]=[C:7]([CH:16]([C:17]2([C:23]3[CH:28]=[CH:27][C:26]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=4)=[CH:25][CH:24]=3)[S:18][CH2:19][CH2:20][CH2:21][S:22]2)[OH:35])[NH:8][CH:9]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86637791HCID 86637791、化合物

生成物 1

HCID 178442243HCID 178442243、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

Step C, 1.5 N Hydrochloric acid (1 mL) was added to a solution of 4-(2,2-dimethylpropyl)-2-{hydroxy[2-(4-pyridin-2-ylphenyl)-1,3-dithian-2-yl]methyl}-N,N-dimethyl-1H-imidazole-1-sulfonamide in tetrahydrofuran (1 mL). After heating in a sealed tube at 70° C. for a few minutes until no further reaction (LCMS), the reaction mixture was cooled to 0° C., quenched with 10% aqueous sodium hydroxide and extracted with ethyl acetate. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo. Preparatory plate chromatography eluting with 10% methanol/ethyl aceate afforded the title compound. LCMS: 440 (M+H).

後処理

  1. temperaturethe reaction mixture was cooled to 0° C.
  2. customquenched with 10% aqueous sodium hydroxide
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined organic extracts were dried (magnesium sulfate)
  5. concentrationconcentrated in vacuo
  6. washPreparatory plate chromatography eluting with 10% methanol/ethyl aceate

出典と根拠

ORDレコード
ord-053bbae116a14252937cbc5c4687260c
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08193228B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート