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Diisopropylethylamine → HCID 58080356, 화합물

HRID 1751801
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HRID 1751801 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 (cf. Liebigs Ann. Chem. 1978.1194) are added. The reaction mixture is heated to 160° C. until there is no further reaction and after cooling it is evaporated to dryness. The residue is mixed with ice water. The product is extracted with dichloromethane and purified by chromatography. 125 mg (III-8) are obtained in the form of a solid. Analytical HPLC-MS (method A): RT=1.08 min.

후처리

  1. customno further reaction
  2. temperatureafter cooling it
  3. customis evaporated to dryness
  4. additionThe residue is mixed with ice water
  5. extractionThe product is extracted with dichloromethane
  6. custompurified by chromatography
  7. custom125 mg (III-8) are obtained in the form of a solid

출처 및 근거

ORD 기록
ord-6dcb647e1595450388ac3a93c09d6baa
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09161927B2

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