Benzyl Alcohol → HCID 59519321、化合物

HRID 237395

反応式

HRID 237395 の反応式
[H-].[Na+].[CH2:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C([O:13][C:14]([C:16]1[S:26][C:19]2[N:20]=[C:21]([NH2:25])[N:22]=[C:23](Cl)[C:18]=2[CH:17]=1)=[O:15])C>C1COCC1>[NH2:25][C:21]1[N:22]=[C:23]([O:10][CH2:3][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[C:18]2[CH:17]=[C:16]([C:14]([OH:15])=[O:13])[S:26][C:19]=2[N:20]=1

参加物

5

反応物 3

HCID 244Benzyl AlcoholHCID 24758Sodium hydrideHCID 16096301Ethyl 2-amino-4-chlorothieno(2,3-d)pyrimidine-6-carboxylate

生成物 1

HCID 59519321HCID 59519321、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
90 °C

実験手順

To a nitrogen filled flask containing sodium hydride (0.5 mmol, 60% in mineral oil) in anhydrous THF (5 ml) was added benzyl alcohol (0.5 mmol). The suspension was stirred vigorously for 10 minutes until no more gas was evolved before being transferred to a microwave reaction tube containing 2-amino-4-chloro-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (0.129 g, 0.5 mmol). The sealed tube was heated to 90° C. for 5 mins using 300 W in a CEM microwave apparatus (CARE!). The reaction mixture was partitioned between DCM and water, the water layer neutralised and evaporated to dryness in vacuo to leave the pure product.

後処理

  1. custombefore being transferred to a microwave reaction tube
  2. customThe reaction mixture was partitioned between DCM and water
  3. customevaporated to dryness in vacuo
  4. customto leave the pure product

出典と根拠

ORDレコード
ord-180ad0c943c64aadac6321cef049ae07
出典データセット
uspto-grants-2014_02
特許番号
US08642594B2

関連ノート

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