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Sodium Hydroxide → HCID 14990622, 화합물

HRID 2166044
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HRID 2166044 반응식
[OH-].[Na+].[OH:3][N:4]1[C:8]2[CH:9]=[C:10]([CH:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[OH:14])[CH:11]=[CH:12][C:7]=2[N:6]=[N:5]1>CO>[CH2:12]([O:3][N:4]1[C:8]2[CH:9]=[C:10]([CH:13]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[OH:14])[CH:11]=[CH:12][C:7]=2[N:6]=[N:5]1)[CH2:7][CH2:8][CH3:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 149906211-hydroxy-alpha-phenyl-1H-benzotriazole-6-methanol

생성물 1

HCID 14990622HCID 14990622, 화합물수율 87.4%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

To a stirred solution of 1.2 parts of sodium hydroxide in 40 parts of methanol were added 7.8 parts of 1-hydroxy-α-phenyl-1H-benzotriazole-6-methanol. After concentration, 18 parts of methylbenzene were added to the concentrate. The solvent was evaporated again and the residue was dissolved in 27 parts of N,N-dimethylformamide. 5.52 Parts of 1-iodobutane were added at once and the whole was stirred for 30 minutes at 50° C. After concentration, 30 parts of water were added. The solidified product was filtered off, washed with water and dissolved in dichloromethane. The organic layer was dried, filtered and evaporated. The residue was crystallized from 17.5 parts of 2,2'-oxybispropane. The product was filtered off and dried, yielding 7.8 parts (87.4%) of 1-butoxy-α-phenyl-1H-benzotriazole-6-methanol; mp. 89.2° C. (int. 65).

후처리

  1. concentrationAfter concentration, 18 parts of methylbenzene
  2. additionwere added to the concentrate
  3. customThe solvent was evaporated again
  4. dissolutionthe residue was dissolved in 27 parts of N,N-dimethylformamide
  5. addition5.52 Parts of 1-iodobutane were added at once and the whole
  6. concentrationAfter concentration, 30 parts of water
  7. additionwere added
  8. filtrationThe solidified product was filtered off
  9. washwashed with water
  10. dissolutiondissolved in dichloromethane
  11. customThe organic layer was dried
  12. filtrationfiltered
  13. customevaporated
  14. customThe residue was crystallized from 17.5 parts of 2,2'-oxybispropane
  15. filtrationThe product was filtered off
  16. customdried

출처 및 근거

ORD 기록
ord-810233fd342b49249f5b38205c0f1d41
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04943574

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