Hydrochloric Acid → HCID 66911325、化合物

HRID 57684ノート

反応式

HRID 57684 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][NH:11]C(=O)OC(C)(C)C)[CH:5]=[CH:4][C:3]=1[C:19]#[N:20].[ClH:21]>O1CCOCC1>[ClH:21].[ClH:21].[NH2:1][C:2]1[C:3]([C:19]#[N:20])=[CH:4][CH:5]=[C:6]([NH:8][CH2:9][CH2:10][NH2:11])[N:7]=1

参加物

4

実験手順

6.76 g (24.38 mmol) of tert-butyl {2-[(6-amino-5-cyanopyridin-2-yl)amino]ethyl}carbamate (Example 29A) were dissolved in 122 ml of a 4N solution of hydrogen chloride in dioxane and the mixture was stirred for 30 min. The reaction mixture was concentrated to half of its original volume and the same amount of diethyl ether was added. The reaction mixture was stirred for 20 min and the product was filtered off and washed with diethyl ether. This gave 5.43 g (89% of theory) of the product as a solid.

後処理

  1. concentrationThe reaction mixture was concentrated to half of its original volume
  2. additionthe same amount of diethyl ether was added
  3. stirringThe reaction mixture was stirred for 20 min
  4. filtrationthe product was filtered off
  5. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-ae72ff823466429994cce794b9ce5191
出典データセット
uspto-grants-2016_09
特許番号
US09434731B2

反応ノート

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