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

HRID 408087ノート

反応式

HRID 408087 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
160 °C

実験手順

1.4 g (II) are placed in 10 ml dioxane, then first 3.6 ml diisopropylethylamine are added followed by 1 g 1-aminocyclopropanemethanol (cf. 8.2). The reaction mixture is heated to 160° C. until there is no further reaction, then cooled and 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 in the form of a solid. Analytical HPLC-MS (method A): RT=1.01 min.

後処理

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

出典と根拠

ORDレコード
ord-9fa898bb4e27488dbf6e0456cb300ff9
出典データセット
uspto-grants-2014_06
特許番号
US08759326B2

反応ノート

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