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Triphenylphosphine → HCID 86610920, 화합물

HRID 2099374
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인쇄 미리보기

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HRID 2099374 반응식
CCOC(/N=N/C(OCC)=O)=O.[OH:13][C@@H:14]1[CH2:19][CH2:18][CH2:17][N:16]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:15]1.[Cl:27][C:28]1[C:37]2[C:32](=[CH:33][C:34](O)=[C:35]([O:38][CH3:39])[CH:36]=2)[N:31]=[CH:30][N:29]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[Cl:27][C:28]1[C:37]2[C:32](=[CH:33][C:34]([O:13][C@H:14]3[CH2:19][CH2:18][CH2:17][N:16]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:15]3)=[C:35]([O:38][CH3:39])[CH:36]=2)[N:31]=[CH:30][N:29]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 1514398(R)-1-Boc-3-hydroxypiperidineHCID 5462977Diethyl azodicarboxylateHCID 1357422514-Chloro-6-methoxyquinazolin-7-ol

생성물 1

HCID 86610920HCID 86610920, 화합물수율 58.6%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

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온도
0 °C

실험 절차

Diethylazodicarboxylate (3.73 g) was added dropwise to a mixture of tert-butyl (3R)-3-hydroxypiperidine-1-carboxylate (4.29 g), 4-chloro-6-methoxyquinazolin-7-ol (3.00 g) and triphenylphosphine (5.61 g) in methylene chloride (75 ml). The solution was then heated to 0° C. and stirred for 3 hours. After cooling the mixture was filtered and then purified by flash column chromatography eluting with isohexane/acetone/triethylamine (80/20/1) to give tert-butyl (3S)-3-[(4-chloro-6-methoxyquinazolin-7-yl)oxy]piperidine-1-carboxylate as a colourless oil (3.29 g) which was used directly; Mass Spectrum: (M+H)+ 394.

후처리

  1. temperatureAfter cooling the mixture
  2. filtrationwas filtered
  3. custompurified by flash column chromatography
  4. washeluting with isohexane/acetone/triethylamine (80/20/1)

출처 및 근거

ORD 기록
ord-4ebe28be436a44bb8399c9b6ca20fe7b
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07569577B2

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