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Diisopropylethylamine → HCID 58080356, 화합물

HRID 405921
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인쇄 미리보기

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HRID 405921 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:22]1([C:25]([OH:28])([CH3:27])[CH3:26])[CH2:24][CH2:23]1>O1CCOCC1>[Cl:1][C:2]1[N:3]=[C:4]([NH:21][C:22]2([C:25]([OH:28])([CH3:27])[CH3:26])[CH2:24][CH2:23]2)[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 12433335HCID 12433335, 화합물HCID 457899672,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine

생성물 1

HCID 58080356HCID 58080356, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
160 °C

실험 절차

2.7 g (II) are placed in 30 ml dioxane, then 6.8 ml diisopropyl-ethylamine and 1.8 g 2-(1-aminocyclopropyl)-propan-2-ol (see Liebigs Ann. Chem. 1978.1194) are added. The reaction mixture is heated to 160° C., until there is no further reaction, and after cooling evaporated to dryness. The residue is combined with ice water. The product is extracted with dichloromethane and purified by chromatography. 125 mg (III-8) are obtained as a solid. Analytical HPLC-MS (method A): RT=1.08 min.

후처리

  1. customno further reaction
  2. temperatureafter cooling
  3. customevaporated to dryness
  4. extractionThe product is extracted with dichloromethane
  5. custompurified by chromatography
  6. custom125 mg (III-8) are obtained as a solid

출처 및 근거

ORD 기록
ord-d8f57d4d709b482082dab0e88b2aa341
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08754073B2

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