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

Hydrochloric Acid → HCID 178443427, 화합물

HRID 1681543
노트
인쇄 미리보기

반응식

HRID 1681543 반응식
[C:1]([CH2:3][C:4]1[CH:5]=[C:6]([CH:20]=[CH:21][C:22]=1[O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])[C:7]([C:9]1[CH:10]=[C:11]([CH:17]=[CH:18][CH:19]=1)[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:8])#[N:2].C([Sn]([N:47]=[N+:48]=[N-:49])(CCCC)CCCC)CCC.Cl.CO>O1CCCC1>[CH2:24]([O:23][C:22]1[CH:21]=[CH:20][C:6]([C:7]([C:9]2[CH:10]=[C:11]([CH:17]=[CH:18][CH:19]=2)[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:8])=[CH:5][C:4]=1[CH2:3][C:1]1[NH:49][N:48]=[N:47][N:2]=1)[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 4984872Tributyltin azideHCID 14739661HCID 14739661, 화합물

생성물 1

HCID 178443427HCID 178443427, 화합물수율 54%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 1.0 g of the product from Example 1 and 2.2 g of tri-n-butylstannylazide in 30 ml of tetrahydrofuran was heated at reflux for 10 days. The reaction was allowed to cool to ambient temperature. A mixture of hydrochloric acid and methanol was added, and after stirring for 30 minutes, the mixture was concentrated in vacuo. The residue was purified by chromatography over silica gel eluting with a 30-75% ethyl acetate in hexane gradient which additionally contained 0.05% acetic acid. The appropriate fractions were cooled and concentrated to provide 592 mg of product. Recrystallization from hexane/ethyl acetate provided 580 mg of the desired title product.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 10 days
  3. additionwas added
  4. concentrationthe mixture was concentrated in vacuo
  5. customThe residue was purified by chromatography over silica gel eluting with a 30-75% ethyl acetate in hexane gradient which additionally contained 0.05% acetic acid
  6. temperatureThe appropriate fractions were cooled
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fa633ea1f04f401e98afac2aa3ad1c3e
출처 데이터셋
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05171882

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트