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

Triethylsilane → HCID 66614157, 화합물

HRID 510137
노트
인쇄 미리보기

반응식

HRID 510137 반응식
COC1C=C(OC)C=CC=1C[N:6]1[C:14](=[O:15])[N:13]([CH2:16][CH2:17][O:18][CH3:19])[C:12]2[C:7]1=[N:8][C:9]([C:20]1[C:28]3[C:23](=[N:24][CH:25]=[CH:26][CH:27]=3)[N:22]([CH2:29][C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[F:36])[N:21]=1)=[N:10][CH:11]=2.C([SiH](CC)CC)C>FC(F)(F)C(O)=O>[F:36][C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=1[CH2:29][N:22]1[C:23]2=[N:24][CH:25]=[CH:26][CH:27]=[C:28]2[C:20]([C:9]2[N:8]=[C:7]3[C:12]([N:13]([CH2:16][CH2:17][O:18][CH3:19])[C:14](=[O:15])[NH:6]3)=[CH:11][N:10]=2)=[N:21]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 12052TriethylsilaneHCID 66614128HCID 66614128, 화합물

생성물 1

HCID 66614157HCID 66614157, 화합물수율 79.5%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

317 mg (0.501 mmol) of the compound from example 83A were dissolved in 15 ml of trifluoroacetic acid, 582 mg (5.009 mmol) of triethylsilane were added and the mixture was heated to reflux for 18 h. The reaction mixture was partitioned between water and ethyl acetate, and neutralized with saturated aqueous sodium hydrogencarbonate solution. The organic phase was dried over sodium sulfate and concentrated on a rotary evaporator. The residue was dried under high vacuum. and purified by means of preparative HPLC (eluent: methanol/water with 0.1% trifluoroacetic acid, gradient 30:70→90:10). 167 mg of the title compound were obtained (79% of theory).

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 18 h
  3. customThe reaction mixture was partitioned between water and ethyl acetate
  4. dry with materialThe organic phase was dried over sodium sulfate
  5. concentrationconcentrated on a rotary evaporator
  6. customThe residue was dried under high vacuum
  7. customand purified by means of preparative HPLC (eluent: methanol/water with 0.1% trifluoroacetic acid, gradient 30:70→90:10)

출처 및 근거

ORD 기록
ord-30536b820a0f4be8bd25b991470062f4
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096592B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트