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Diisopropylethylamine → (5S)-5-[(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)amino]-1-methyl-2-piperidinone

HRID 518028
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반응식

HRID 518028 반응식
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1.C(N(C(C)C)CC)(C)C.[NH2:21][C@@H:22]1[CH2:27][N:26]([CH3:28])[C:25](=[O:29])[CH2:24][CH2:23]1>O1CCOCC1>[Cl:1][C:2]1[N:3]=[C:4]([NH:21][C@@H:22]2[CH2:27][N:26]([CH3:28])[C:25](=[O:29])[CH2:24][CH2:23]2)[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1
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참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 28064098HCID 28064098, 화합물HCID 457899672,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine

생성물 1

HCID 59708467(5S)-5-[(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)amino]-1-methyl-2-piperidinone

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
130 °C

실험 절차

0.27 g (II) are placed in 3 ml dioxane, then 0.45 ml diisopropylethylamine and 0.25 g (S)-5-amino-1-methylpiperidin-2-one are added. The reaction mixture is heated to 130° C. until no further reaction takes place, then cooled and evaporated down. The product is extracted with dichloromethane and purified by chromatography (preparative HPLC, method B). 0.26 g (III-5) are obtained as a solid. Analytical HPLC-MS (method A): RT=1.06 min.

후처리

  1. temperaturecooled
  2. customevaporated down
  3. extractionThe product is extracted with dichloromethane
  4. custompurified by chromatography (preparative HPLC, method B)
  5. custom0.26 g (III-5) are obtained as a solid

출처 및 근거

ORD 기록
ord-6912134426444515a057807e0c7c4bcf
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115142B2

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