(4-Methoxy-benzyl)-[4-methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-yl]-amine → 4-Methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-ylamine

HRID 1951192ノート

反応式

HRID 1951192 の反応式
COC1C=CC(C[NH:8][C:9]2[S:10][C:11]([C:15]3[CH:20]=[CH:19][N:18]=[C:17]([N:21]4[CH2:26][CH2:25][O:24][CH2:23][CH2:22]4)[N:16]=3)=[C:12]([CH3:14])[N:13]=2)=CC=1>FC(F)(F)C(O)=O.O>[CH3:14][C:12]1[N:13]=[C:9]([NH2:8])[S:10][C:11]=1[C:15]1[CH:20]=[CH:19][N:18]=[C:17]([N:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[N:16]=1

参加物

3

反応物 1

HCID 86610335(4-Methoxy-benzyl)-[4-methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-yl]-amine

生成物 1

HCID 866103364-Methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-ylamine

試薬・触媒・溶媒 1

HCID 22392675Trifluoroacetic acid water溶媒

反応条件

温度
75 °C

実験手順

A solution comprising (4-methoxy-benzyl)-[4-methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-yl]-amine (25c) (0.45 g, 1.13 mmol) in trifluoroacetic acid:water (95:5) (10 ml) is heated at 75° C. for days. The solvent is removed in vacuo and the crude residue is dissolved in ethyl acetate. The pH is adjusted to pH12 using 2N sodium hydroxide and the layers are separated. The aqueous layer is extracted with ethyl acetate (2×30 ml). The organic portions are combined and washed with brine (50 ml), dried over MgSO4 and concentrated in vacuo to yield the titled compound as a brown solid.

後処理

  1. customThe solvent is removed in vacuo
  2. dissolutionthe crude residue is dissolved in ethyl acetate
  3. customthe layers are separated
  4. extractionThe aqueous layer is extracted with ethyl acetate (2×30 ml)
  5. washwashed with brine (50 ml)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8c7f8a191e05474a866482fb25528157
出典データセット
uspto-grants-2013_03
特許番号
US08404684B2

反応ノート

読み込み中…