Triphenylphosphine → HCID 46836199, 화합물

HRID 474212노트

반응식

HRID 474212 반응식
[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

참가 물질

6

반응물 4

HCID 11776Triphenylphosphine2회HCID 97268Di-tert-butyl azodicarboxylate2회HCID 100165Cyclopentane-1,3-diolHCID 59438049HCID 59438049, 화합물

생성물 1

HCID 46836199HCID 46836199, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e9eb59344b0d42c0b317ad287184d618
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637518B2

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