홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Hydrochloric Acid → 5-Chloro-3-(2-tritylamino-3-hydroxypropoxy)-1,2-benzoisoxazole

HRID 1901600
노트
인쇄 미리보기

반응식

HRID 1901600 반응식
[C:1](Cl)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:21][CH:22]([CH2:35][OH:36])[CH2:23][O:24][C:25]1[C:29]2[CH:30]=[C:31]([Cl:34])[CH:32]=[CH:33][C:28]=2[O:27][N:26]=1.C(N(CC)CC)C.Cl>CN(C)C=O.C(OCC)(=O)C>[Cl:34][C:31]1[CH:32]=[CH:33][C:28]2[O:27][N:26]=[C:25]([O:24][CH2:23][CH:22]([NH:21][C:1]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:35][OH:36])[C:29]=2[CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 153825803-(2-Amino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole

생성물 1

HCID 233684925-Chloro-3-(2-tritylamino-3-hydroxypropoxy)-1,2-benzoisoxazole

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

A solution of 5.58 g of trityl chloride in 6 ml of N,N-dimethylformamide is added to a solution of 4.85 g of 3-(2-amino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole and 2.02 g of triethylamine in 12 ml of N,N-dimethylformamide at -40° to -30° C., and they are subjected to reaction at the same temperature for 30 minutes. Subsequently, ice water and ethyl acetate are added to the reaction mixture and the pH is adjusted to 2 with 2N hydrochloric acid. The organic layer is separated, and the separated organic layer is washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure. The residue obtained is crystallized from n-hexane and the crystals are collected by filtration, to obtain 7.28 g of colorless, crystalline 5-chloro-3-(2-tritylamino-3-hydroxypropoxy)-1,2-benzoisoxazole having a melting point of 142°-144° C.

후처리

  1. customthey are subjected to reaction at the same temperature for 30 minutes
  2. customThe organic layer is separated
  3. washthe separated organic layer is washed with a saturated saline solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customafter which the solvent is removed by distillation under reduced pressure
  6. customThe residue obtained
  7. customis crystallized from n-hexane
  8. filtrationthe crystals are collected by filtration

출처 및 근거

ORD 기록
ord-ca787c46f3524ff7b57cd5a82caa3689
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05578627

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트