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Dimethyl Sulfoxide → 5-Tert-butylpyridine-3-carbaldehyde

HRID 2071081
ノート
印刷プレビュー

反応式

HRID 2071081 の反応式
C(Cl)(=O)C(Cl)=O.CS(C)=O.[C:11]([C:15]1[CH:16]=[C:17]([CH2:21][OH:22])[CH:18]=[N:19][CH:20]=1)([CH3:14])([CH3:13])[CH3:12].C(N(CC)CC)C>C(Cl)Cl>[C:11]([C:15]1[CH:20]=[N:19][CH:18]=[C:17]([CH:16]=1)[CH:21]=[O:22])([CH3:14])([CH3:12])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 53779320(5-(tert-Butyl)pyridin-3-yl)methanol

生成物 1

HCID 595699785-Tert-butylpyridine-3-carbaldehyde

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Oxalyl chloride (158 μL, 1.819 mmol) in methylene chloride (10 mL) was placed in a two-necked flask at −78° C., followed by the addition of dimethyl sulfoxide (129 μL, 1.819 mmol). Stirring was continued for 20 min, followed by addition of (5-tert-butylpyridin-3-yl)methanol (0.2 g, 1.21 mmol) in methylene chloride (10 mL). After the mixture was stirred at −78° C. for additional 20 min, triethylamine (0.59 mL, 4.24 mmol) was added. The cooling bath was removed and the suspension was allowed to warm to room temperature. Water (50 mL) was added, the yellow organic layer was separated, and the aqueous layer was extracted with methylene chloride (3×30 mL). The combined organic solution was dried and concentrated to give 5-tert-butylnicotinaldehyde as an orange-yellow liquid which was used directly for next step without further purification.

後処理

  1. stirringAfter the mixture was stirred at −78° C. for additional 20 min
  2. customThe cooling bath was removed
  3. additionWater (50 mL) was added
  4. customthe yellow organic layer was separated
  5. extractionthe aqueous layer was extracted with methylene chloride (3×30 mL)
  6. customThe combined organic solution was dried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-c057b322682f44368de96eb2ed4d5f3f
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08299267B2

反応ノート

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