Triphenylphosphine → HCID 46836199、化合物

HRID 474212ノート

反応式

HRID 474212 の反応式
[OH:1][C:2]1[CH:3]=[N:4][C:5]([C:8]2[CH:9]=[C:10]([CH:25]=[CH:26][CH:27]=2)[CH2:11][N:12]2[C:17](=[O:18])[CH:16]=[CH:15][C:14]([C:19]3[CH:20]=[N:21][N:22]([CH3:24])[CH:23]=3)=[N:13]2)=[N:6][CH:7]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH:47]1(O)[CH2:51][CH2:50][CH:49]([OH:52])[CH2:48]1.N(C(OC(C)(C)C)=O)=NC(OC(C)(C)C)=O>CN(C=O)C>[OH:52][CH:49]1[CH2:50][CH2:51][CH:47]([O:1][C:2]2[CH:3]=[N:4][C:5]([C:8]3[CH:9]=[C:10]([CH:25]=[CH:26][CH:27]=3)[CH2:11][N:12]3[C:17](=[O:18])[CH:16]=[CH:15][C:14]([C:19]4[CH:20]=[N:21][N:22]([CH3:24])[CH:23]=4)=[N:13]3)=[N:6][CH:7]=2)[CH2:48]1

参加物

6

反応物 4

HCID 11776Triphenylphosphine2 回HCID 97268Di-tert-butyl azodicarboxylate2 回HCID 100165Cyclopentane-1,3-diolHCID 59438049HCID 59438049、化合物

生成物 1

HCID 46836199HCID 46836199、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

100 mg (0.28 mmol) of 2-[3-(5-hydroxypyrimidin-2-yl)benzyl]-6-(1-methyl-1H-pyrazol-4-yl)-2H-pyridazin-3-one are dissolved in 6 ml of DMF, and 277 mg (0.83 mmol) of polymer-bound triphenylphosphine (3 mmol/g) and 33 mg (0.32 mmol) of 1,3-cyclopentanediol are added. The reaction mixture is shaken at room temperature for 15 min, and 196 mg (0.83 mmol) of di-tert-butyl azodicarboxylate are subsequently added. The reaction mix-ture was shaken at room temperature for 3 h, a further 277 mg (0.83 mmol) of polymer-bound triphenylphosphine (3 mmol/g) and 196 mg (0.83 mmol) of di-tert-butyl azodicarboxylate were added, and the mixture was shaken at room temperature for 18 h. The reaction mixture is filtered off through kieselguhr with suction and washed with acetonitrile. The filtrate is evaporated and purified by means of preparative HPLC.

後処理

  1. additionThe reaction mix-ture
  2. stirringwas shaken at room temperature for 3 h
  3. stirringthe mixture was shaken at room temperature for 18 h
  4. filtrationThe reaction mixture is filtered off through kieselguhr with suction
  5. washwashed with acetonitrile
  6. customThe filtrate is evaporated
  7. custompurified by means of preparative HPLC

出典と根拠

ORDレコード
ord-e9eb59344b0d42c0b317ad287184d618
出典データセット
uspto-grants-2014_01
特許番号
US08637518B2

反応ノート

読み込み中…