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

Nitrogen → 1-(Tert-butoxycarbonyl)indole

HRID 2078687
노트
인쇄 미리보기

반응식

HRID 2078687 반응식
[C:1]([O:5][C:6]([N:8]1[C:12]2[CH:13]=[CH:14]S[C:11]=2[C:10](I)=N1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:17](=O)([O-])[O-].[K+].[K+].N#N.O1CC[CH2:27][CH2:26]1>C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:1]([O:5][C:6]([N:8]1[C:12]2[C:11](=[CH:10][CH:17]=[CH:14][CH:13]=2)[CH:27]=[CH:26]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 947NitrogenHCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 57637299tert-Butyl 3-iodo-1H-thieno[3,2-c]pyrazole-1-carboxylate

생성물 1

HCID 35329801-(Tert-butoxycarbonyl)indole수율 69%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 8857Ethyl Acetate용매

반응 조건

온도
57.5 °C

실험 절차

A mixture of 5-(tert-butyl-dimethyl-silanyloxymethyl)-1H-indole-2-boronic acid 1-carboxylic acid tert-butyl ester [3.82 g, 9.42 mmol, Intermediate (8), prepared as described in Example 1-4 of International Patent Application Publication No. WO 02/32861], 3-iodo-thieno[3,2-c]pyrazole-1-carboxylic acid tert-butyl ester [4.0 g, 11.42 mmol, Example 5B above], tetrakis(triphenylphosphine)palladium(0) (544 mg, 0.470 mmol), potassium carbonate (2M aqueous, 12 mL) in tetrahydrofuran (60 mL) is purged with N2 for 10 minutes then heated to 55-60° C. for 7.5 hours. The reaction is diluted with ethyl acetate (50 mL) and washed with water (20 mL). Water layer is back extracted with ethyl acetate (50 mL). The combined ethyl acetate phases are dried over sodium sulfate. The residue is chromatographed on 35 g silica gel cartridge (5-30% ethyl acetate gradient in heptane) to give 2-(1-tert-butoxycarbonyl-1H-thieno[3,2-c]pyrazol-3-yl)-5-tert-butyl-dimethyl-silanyloxymethyl)-indole-1-carboxlic acid tert-butyl ester [3.8 g, 69%, Intermediate (9)]; 1H NMR [(CD3)2SO)]: δ 8.08 (2H, m), 7.64 (1H, s), 7.38 (2H, m), 7.14 (1H, s), 4.81 (2H, s, —OCH), 1.65 (9H, s), 1.32 (9H, s), 0.92 (9H, s, Si(CH3)3), 0.10 (6H, s, Si(CH2)); LC/MS: 584 (M+H).

후처리

  1. customprepared
  2. washwashed with water (20 mL)
  3. extractionWater layer is back extracted with ethyl acetate (50 mL)
  4. dry with materialThe combined ethyl acetate phases are dried over sodium sulfate
  5. customThe residue is chromatographed on 35 g silica gel cartridge (5-30% ethyl acetate gradient in heptane)

출처 및 근거

ORD 기록
ord-f3188e6a250b42d987308ab3300ed689
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07928231B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트