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

Triethylamine → HCID 136121371, 화합물

HRID 2062303
노트
인쇄 미리보기

반응식

HRID 2062303 반응식
[O:1]1[CH2:5][CH2:4][CH2:3][C@@H:2]1[C:6]([OH:8])=O.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:33][CH:34]1[CH2:39][CH2:38][N:37]([C:40]2[C:49]3[C:44](=[CH:45][C:46]([CH3:50])=[CH:47][CH:48]=3)[N:43]=[C:42]([C:51]3[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=3[OH:57])[N:41]=2)[CH2:36][CH2:35]1.C(N(CC)CC)C>CN(C=O)C>[OH:57][C:52]1[CH:53]=[CH:54][CH:55]=[CH:56][C:51]=1[C:42]1[N:41]=[C:40]([N:37]2[CH2:36][CH2:35][CH:34]([NH:33][C:6]([C@H:2]3[CH2:3][CH2:4][CH2:5][O:1]3)=[O:8])[CH2:39][CH2:38]2)[C:49]2[C:44](=[CH:45][C:46]([CH3:50])=[CH:47][CH:48]=2)[N:43]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 2734707Tetrahydro-2-furoic acid, (+)-HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 136104957HCID 136104957, 화합물

생성물 1

HCID 136121371HCID 136121371, 화합물수율 42.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

(R)-Tetrahydrofuran-2-carboxylic acid (193 mg, 1.66 mmol) was dissolved in DMF (6 mL), followed by the addition of HATU (696 mg, 1.83 mmol). The mixture was then stirred for 15 min at room temperature under an N2 atmosphere. The 2-[4-(4-Amino-piperidin-1-yl)-7-methyl-quinazolin-2-yl]-phenol (556 mg, 1.66 mmol) was dissolved in DMF (8 mL) and added to the mixture, followed by triethylamine (336 mg, 0.463 mL, 3.32 mmol). After 30 min, the DMF was removed in vacuo and the crude product partitioned between water and ethyl acetate. The aqueous layer was separated, washed with ethyl acetate, and the combined organic layers dried over MgSO4, filtered, and concentrated to give crude product as an orange oil. Purification via silica gel chromatography (20% ethyl acetate/80% 1:1 CH2Cl2:hexane) gave pure (R)-Tetrahydro-furan-2-carboxylic acid {1-[2-(2-hydroxy-phenyl)-7-methyl-quinazolin-4-yl]-piperidin-4-yl}-amide (303 mg, 42%). 1H NMR (400 MHz, DMSO-d6) δ 8.44 (dd, J=8.2, 1.5 Hz, 1H), 7.90 (d, J=8.5 Hz, 1H), 7.75 (d, J=8.3 Hz, 1H), 7.67 (s, 1H), 7.40-7.36 (m, 2H), 6.97-6.93 (m, 2H), 4.48-4.45 (m, 2H), 4.20 (dd, J=8.2, 5.3 Hz, 1H), 4.06-3.96 (m, 1H), 3.88 (dd, J=14.3, 6.6 Hz, 1H), 3.74 (dd, J=14.5, 6.7 Hz, 1H), 3.43-3.32 (m, 2H), 2.51 (s, 3H), 2.16-2.07 (m, 1H), 1.89-1.69 (m, 7H). 13C NMR (100 MHz, DMSO-d6) δ 171.7, 162.8, 160.7, 159.5, 149.3, 144.1, 132.5, 129.0, 127.3, 125.7, 125.4, 118.9, 118.4, 117.2, 111.9, 77.6, 68.5, 48.3, 45.5, 31.3, 31.2, 30.0, 24.9, 21.2.

후처리

  1. additionadded to the mixture
  2. waitAfter 30 min
  3. customthe DMF was removed in vacuo
  4. customthe crude product partitioned between water and ethyl acetate
  5. customThe aqueous layer was separated
  6. washwashed with ethyl acetate
  7. dry with materialthe combined organic layers dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customto give crude product as an orange oil
  11. customPurification via silica gel chromatography (20% ethyl acetate/80% 1:1 CH2Cl2:hexane)

출처 및 근거

ORD 기록
ord-0419b77d000640ada435a36312eb777f
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08283354B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트