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4-Hydroxybiphenyl → HCID 59759083, 화합물

HRID 914517
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인쇄 미리보기

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HRID 914517 반응식
[OH:1][CH2:2][CH2:3][C:4]1[N:5]=[C:6]([S:9][C:10]([CH3:15])([CH3:14])[C:11]([OH:13])=[O:12])[S:7][CH:8]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:35]1([C:41]2[CH:46]=[CH:45][C:44](O)=[CH:43][CH:42]=2)[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>O1CCCC1>[C:35]1([C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[CH:40]=[CH:39][C:38]([O:1][CH2:2][CH2:3][C:4]2[N:5]=[C:6]([S:9][C:10]([CH3:15])([CH3:14])[C:11]([OH:13])=[O:12])[S:7][CH:8]=2)=[CH:37][CH:36]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 71034-HydroxybiphenylHCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 67396216HCID 67396216, 화합물

생성물 1

HCID 59759083HCID 59759083, 화합물수율 3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

To a suspension of 2-{[4-(2-hydroxyethyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid resin (0.3 g) synthesized in Example 713-1 in tetrahydrofuran (3.0 mL) were added triphenylphosphine (0.12 g) and 4-phenylphenol (0.17 g), and the mixture was left standing for 15 min. Thereto was added diisopropyl azodicarboxylate (40% toluene solution, 0.26 ml), and the mixture was stirred at room temperature for 30 min. The resin was collected by filtration from the reaction mixture, and washed three times with tetrahydrofuran. This operation was repeated three times, and the obtained resin was washed three times each with dimethylformamide, tetrahydrofuran and methanol, and vacuum dried. To the resin was added trifluoroacetic acid, and the mixture was left standing at room temperature for 4 hr. The resin was filtered off and the filtrate was concentrated by blowing nitrogen gas thereto, and purified by HPLC to give the title compound (0.012 g) as a colorless oil.

후처리

  1. waitthe mixture was left
  2. filtrationThe resin was collected by filtration from the reaction mixture
  3. washwashed three times with tetrahydrofuran
  4. washthe obtained resin was washed three times each with dimethylformamide, tetrahydrofuran and methanol, and vacuum
  5. customdried
  6. additionTo the resin was added trifluoroacetic acid
  7. waitthe mixture was left
  8. waitstanding at room temperature for 4 hr
  9. filtrationThe resin was filtered off
  10. concentrationthe filtrate was concentrated
  11. custompurified by HPLC

출처 및 근거

ORD 기록
ord-1ff89335f1084edd922951641d18654e
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08026370B2

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