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

Diisopropylethylamine → HCID 59619453, 화합물

HRID 1367514
노트
인쇄 미리보기

반응식

HRID 1367514 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C@@H:11]2[CH2:15][C@@H:14]([C:16](O)=[O:17])[C@H:13]([C:19]([N:21]3[CH2:24][C:23]([F:26])([F:25])[CH2:22]3)=[O:20])[CH2:12]2)(=[O:10])=[O:9])=[C:4]([C:27]([F:30])([F:29])[F:28])[CH:3]=1.C(N(CC)C(C)C)(C)C.C[NH3+].F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)[C:53]2[N:54]=C[CH:56]=[CH:57][C:52]=2[N:51]=N1.F[P-](F)(F)(F)(F)F.C1C(N)(C#N)C1.Cl>C(#N)C>[C:53]([C:52]1([NH:51][C:16]([C@@H:14]2[CH2:15][C@@H:11]([S:8]([C:5]3[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=3[C:27]([F:29])([F:30])[F:28])(=[O:10])=[O:9])[CH2:12][C@H:13]2[C:19]([N:21]2[CH2:22][C:23]([F:25])([F:26])[CH2:24]2)=[O:20])=[O:17])[CH2:56][CH2:57]1)#[N:54]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 145863631-Amino-1-cyclopropanecarbonitrile hydrochlorideHCID 866211442-(1H-7-Azabenzotriazol-1-yl)-1,1,3,3-tetramethyl uronium hexafluorophosphate MethanaminiumHCID 86649026HCID 86649026, 화합물

생성물 1

HCID 59619453HCID 59619453, 화합물수율 85%

시약·촉매·용매

1
HCID 6342Acetonitrile용매

실험 절차

To a mixture of (1R,2R,4S)-4-(4-Bromo-2-trifluoromethyl-benzenesulfonyl)-2-(3,3-difluoro-azetidine-1-carbonyl)-cyclopentanecarboxylic acid (150 mg, 0.29 mmol), N,N-diisopropylethylamine (0.15 mL, 0.87 mmol), 2-(1H-7-Azabenzotriazol-1-yl)-1,1,3,3-tetramethyl uronium hexafluorophosphate methanaminium (221 mg, 0.58 mmol) in acetonitrile was added 1-amino-cyclopropyl cyanic hydrochloride (41 mg, 0.34 mmol). The reaction mixture was stirred at room temperature for 16 h then concentrated in vacuo and partitioned between ethyl acetate and an aqueous solution of sodium carbonate (5% w/w). The aqueous layer was extracted with ethyl acetate then the combined organic layers were washed with aqueous hydrochloric acid (1N) and brine then dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash chromatography on silica gel with a gradient of dichloromethane/methanol (98:2 v/v) as eluant to afford the title compound (144 mg, 85%) as a brown solid. MS (EI): 584.0 (M−H)−.

후처리

  1. concentrationthen concentrated in vacuo
  2. custompartitioned between ethyl acetate
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. washthe combined organic layers were washed with aqueous hydrochloric acid (1N) and brine
  5. dry with materialthen dried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash chromatography on silica gel with a gradient of dichloromethane/methanol (98:2 v/v) as eluant

출처 및 근거

ORD 기록
ord-709e4a2601904c6bb3ed54a1625e74b0
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07893099B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트