Diisopropylethylamine → [1-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)-cyclopropyl]-methanol

HRID 1529507노트

반응식

HRID 1529507 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([CH2:25][OH:26])[CH2:24][CH2:23]1>O1CCOCC1>[Cl:1][C:2]1[N:3]=[C:4]([NH:21][C:22]2([CH2:25][OH:26])[CH2:24][CH2:23]2)[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 14146220(1-Aminocyclopropyl)methanolHCID 457899672,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine

생성물 1

HCID 59708441[1-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)-cyclopropyl]-methanol

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
160 °C

실험 절차

1.4 g (II) are placed in 10 ml dioxane, then 3.6 ml diisopropylethylamine followed by 1 g of 1-aminocyclopropanemethanol (see 4.2) are added. The reaction mixture is heated at 160° C. until there is no further reaction, and after cooling evaporated down. The residue is treated with cyclohexane/ethyl acetate (8:2) in the ultrasound bath and the solid is suction filtered and dried. 1.24 g (III-4) are obtained as a solid.

후처리

  1. additionare added
  2. customno further reaction
  3. temperatureafter cooling
  4. customevaporated down
  5. additionThe residue is treated with cyclohexane/ethyl acetate (8:2) in the ultrasound bath
  6. filtrationfiltered
  7. customdried
  8. custom1.24 g (III-4) are obtained as a solid

출처 및 근거

ORD 기록
ord-633eb96f63ca4b6082c580e68398b606
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09090626B2

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