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Acetic Anhydride → 1-Acetoxymethyl-2-(4-methoxy-2-picolylmercapto)-1H-thieno[3,4-d]imidazole

HRID 231166
ノート
印刷プレビュー

反応式

HRID 231166 の反応式
[OH:1][CH2:2][N:3]1[C:7]2=[CH:8][S:9][CH:10]=[C:6]2[N:5]=[C:4]1[S:11][CH2:12][C:13]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][N:14]=1.[C:21](OC(=O)C)(=[O:23])[CH3:22]>N1C=CC=CC=1.CN(C)C1C=CN=CC=1>[C:21]([O:1][CH2:2][N:3]1[C:7]2=[CH:8][S:9][CH:10]=[C:6]2[N:5]=[C:4]1[S:11][CH2:12][C:13]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][N:14]=1)(=[O:23])[CH3:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 141543311-Hydroxymethyl-2-(4-methoxy-2-picolylmercapto)1H-thieno[3,4-d]imidazole

生成物 1

HCID 141543321-Acetoxymethyl-2-(4-methoxy-2-picolylmercapto)-1H-thieno[3,4-d]imidazole

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

1.3 g (4.2 mmol) of the title compound from Example 28 were dissolved in 25 ml of anhydrous pyridine, and 50 mg of 4-dimethylaminopyridine were added. Under a nitrogen atmosphere and while stirring, 6.3 ml acetic anhydride were added dropwise, and the mixture was stirred at room temperature for one hour. It was then poured onto ice water, extracted with methylene chloride, and the organic phase was dried over MgSO4 and concentrated in vacuo. The crystalline solid was recrystallized from ethanol. Melting point 111°-113° C.

後処理

  1. stirringthe mixture was stirred at room temperature for one hour
  2. additionIt was then poured onto ice water
  3. extractionextracted with methylene chloride
  4. dry with materialthe organic phase was dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe crystalline solid was recrystallized from ethanol

出典と根拠

ORDレコード
ord-78a64d4ef68b4ee0999c8357f465b6ba
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04845118

反応ノート

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