Trifluoroacetic acid → N-(3-(2-Fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamide

HRID 530888노트

반응식

HRID 530888 반응식
[F:1][C:2]1[CH:55]=[CH:54][CH:53]=[CH:52][C:3]=1[CH2:4][C:5]1([CH2:49][O:50][CH3:51])[CH2:10][CH2:9][CH2:8][N:7]([NH:11][C:12]([C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[N:19](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[N:18]=[C:17]3[C:42]2[CH:47]=[CH:46][N:45]=[C:44]([CH3:48])[CH:43]=2)=[O:13])[CH2:6]1.FC(F)(F)C(O)=O.C([SiH](CC)CC)C>>[F:1][C:2]1[CH:55]=[CH:54][CH:53]=[CH:52][C:3]=1[CH2:4][C:5]1([CH2:49][O:50][CH3:51])[CH2:10][CH2:9][CH2:8][N:7]([NH:11][C:12]([C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[NH:19][N:18]=[C:17]3[C:42]2[CH:47]=[CH:46][N:45]=[C:44]([CH3:48])[CH:43]=2)=[O:13])[CH2:6]1

참가 물질

4

반응물 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 68074196N-(3-(2-Fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxamide

생성물 1

HCID 67985892N-(3-(2-Fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1H-indazole-5-carboxamide

실험 절차

In a flask, N-(3-(2-fluorobenzyl)-3-(methoxymethyl)piperidin-1-yl)-3-(2-methylpyridin-4-yl)-1-trityl-1H-indazole-5-carboxamide (crude, from previous step) was reacted with trifluoroacetic acid (3 mL) for 1 hour. After reaction completion triethylsilane (0.1 mL) was added, and the reaction was stirred for an additional 15 minutes. The reaction was concentrated and rinsed with diethyl ether. The resulting remaining precipitate was dried and further purified using HPLC to give the titled compound. LC-MS: 488.24 [M+H]. LC/MS RT=2.49 min.

후처리

  1. additionwas added
  2. concentrationThe reaction was concentrated
  3. washrinsed with diethyl ether
  4. customThe resulting remaining precipitate was dried
  5. customfurther purified

출처 및 근거

ORD 기록
ord-40c27145af0f46938c98a5616f52a313
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09351965B2

반응 노트

불러오는 중…