Benzyl Alcohol → HCID 59519321, 화합물

HRID 237395

반응식

HRID 237395 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 59519321HCID 59519321, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-180ad0c943c64aadac6321cef049ae07
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642594B2

연결된 노트

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