Hydrazine hydrate (1:1) → (2-Chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methanamine

HRID 1365122ノート

反応式

HRID 1365122 の反応式
[Cl:1][C:2]1[N:3]=[C:4]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)[C:5]2[S:10][C:9]([CH2:11][N:12]3C(=O)C4C(=CC=CC=4)C3=O)=[CH:8][C:6]=2[N:7]=1.NN.O>CO>[Cl:1][C:2]1[N:3]=[C:4]([N:23]2[CH2:24][CH2:25][O:26][CH2:27][CH2:28]2)[C:5]2[S:10][C:9]([CH2:11][NH2:12])=[CH:8][C:6]=2[N:7]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 595931082-((2-Chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methyl)isoindoline-1,3-dione

生成物 1

HCID 46180727(2-Chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methanamine収率 73.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 2-((2-chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methyl)isoindoline-1,3-dione 31 (100 mg, 0.24 mmol) in MeOH (7 mL) was added H2NNH2.H2O (24 μL, 0.48 mmol). The reaction was heated at reflux for 1 h. After cooling to room temperature the reaction was quenched with water (10 mL) and extracted with EtOAc. The combined organics were dried over Na2SO4 and concentrated in vacuo to afford (2-chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methanamine 27 (0.05 g, 73%). MS (Q1) 285 (M)+

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 1 h
  3. customwas quenched with water (10 mL)
  4. extractionextracted with EtOAc
  5. dry with materialThe combined organics were dried over Na2SO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-d9bb846c32de498aa3f8f8fe3184e497
出典データセット
uspto-grants-2011_02
特許番号
US07888352B2

反応ノート

読み込み中…