1,2-Dichloroethane → HCID 59640537、化合物

HRID 2250141ノート

反応式

HRID 2250141 の反応式
[N:1]1([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3([NH2:20])[CH2:19][CH2:18]3)=[CH:13][CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[N:21]1([CH2:27][C:28](O)=[O:29])[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1.C(N(C(C)C)CC)(C)C.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C>[N:21]1([CH2:27][C:28]([NH:20][C:17]2([C:14]3[CH:13]=[CH:12][C:11]([O:10][CH2:9][CH2:8][CH2:7][N:1]4[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]4)=[CH:16][CH:15]=3)[CH2:18][CH2:19]2)=[O:29])[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 4389684-Morpholineacetic acidHCID 59640425HCID 59640425、化合物

生成物 1

HCID 59640537HCID 59640537、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1-[4-(3-Piperidin-1-yl-propoxy)-phenyl]-cyclopropylamine (0.195 g, 0.72 mmol) and morpholin-4-yl-acetic acid (0.125 g, 0.86 mmol) are dissolved in DMF, and diisopropylethylamine added (0.15 mL), followed by EDC (0.165 g, 0.86 mmol) and HOBt (0.116 g, 0.86 mmol). The reaction mixture was stirred overnight at room temperature. The residue is purified by chromatography [SCX-MeOH wash, elute 2M NH3/MeOH; then Biotage 12M SiO2, elute 10% (25/5/1 CHCl3/MeOH/NH4OH)/90% (10% MeOH/CHCl3)] to give the title compound as a yellow oil. HRMS 402.2765 (M+H)+.

後処理

  1. customThe residue is purified by chromatography [SCX-MeOH
  2. washwash
  3. washelute 2M NH3/MeOH
  4. washthen Biotage 12M SiO2, elute 10% (25/5/1 CHCl3/MeOH/NH4OH)/90% (10% MeOH/CHCl3)]

出典と根拠

ORDレコード
ord-8cb01932ff8e4256a04d85fd1549fc02
出典データセット
uspto-grants-2008_01
特許番号
US07314937B2

反応ノート

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