Diisopropylethylamine → HCID 59708411, compound

HRID 330874Notes

Reaction equation

HRID 330874 reaction equation
[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][CH:22]1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1>O1CCOCC1>[Cl:1][C:2]1[N:3]=[C:4]([NH:21][CH:22]2[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1

Participants

5

Conditions

Temperature
130 °C

Procedure

0.68 g (II) are placed in 6 ml dioxane, then 1.72 ml diisopropylethylamine followed by 0.6 g 4-aminotetrahydropyran are added. The reaction mixture is heated to 130° C. until there is no further reaction and after cooling evaporated down. The product is treated with water in the ultrasound bath and the solid is suction filtered and dried. 0.66 g (III-3) are obtained. Analytical HPLC-MS (method A): RT=1.08 min.

Workup

  1. additionare added
  2. customno further reaction
  3. temperatureafter cooling
  4. customevaporated down
  5. additionThe product is treated with water in the ultrasound bath
  6. filtrationfiltered
  7. customdried
  8. custom0.66 g (III-3) are obtained

Sources & evidence

ORD record
ord-5322f4e621a349ed8072ef846b90e7c9
Source dataset
uspto-grants-2014_11
Patent number
US08877758B2

Reaction notes

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