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

Phosphate → HCID 67822659, 화합물

HRID 1492466
노트
인쇄 미리보기

반응식

HRID 1492466 반응식
[H-].[Li+].[NH2:3][C:4]1[N:12]=[C:11]2[C:7]([NH:8][CH:9]=[N:10]2)=[C:6]([O:13][CH2:14][CH2:15][O:16][CH3:17])[N:5]=1.CS(O[C@H:23]1[CH2:27][CH2:26][C@H:25]([CH2:28][O:29][Si:30]([C:43]([CH3:46])([CH3:45])[CH3:44])([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C@H:24]1[CH2:47][O:48][Si:49]([C:62]([CH3:65])([CH3:64])[CH3:63])([C:56]1[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=1)[C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1)(=O)=O.P([O-])([O-])([O-])=O>CN(C=O)C.CO>[NH2:3][C:4]1[N:12]=[C:11]2[C:7]([N:8]=[CH:9][N:10]2[C@@H:23]2[CH2:27][CH2:26][C@H:25]([CH2:28][O:29][Si:30]([C:43]([CH3:45])([CH3:44])[CH3:46])([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)[C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)[C@H:24]2[CH2:47][O:48][Si:49]([C:62]([CH3:65])([CH3:64])[CH3:63])([C:50]2[CH:51]=[CH:52][CH:53]=[CH:54][CH:55]=2)[C:56]2[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=2)=[C:6]([O:13][CH2:14][CH2:15][O:16][CH3:17])[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1061PhosphateHCID 62714Lithium hydrideHCID 135468096-(2-Methoxyethoxy)-7H-purin-2-amineHCID 88444072HCID 88444072, 화합물

생성물 1

HCID 67822659HCID 67822659, 화합물수율 29%

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 6228Dimethylformamide용매

실험 절차

In an atmosphere of argon gas, lithium hydride (8.4 mg, 1.06 mmoles) was added to a suspension of 2-amino-6-(2-methoxyethoxy)purine (221 mg, 1.06 mmoles) in DMF (7 ml). After stirring the mixture for one hour, (1S,2S,3S)-2,3-bis(t-butyldiphenylsilyloxymethyl)-1-cyclopentyl methanesulfonate (370 mg, 0.53 mmole) was added, and the resulting mixture was stirred at 140° C. for one hour. After cooling the mixture, 0.2M phosphate buffer (pH 7) was added, and the product formed was extracted with ethyl acetate. The extract solution was washed with water, washed with saturated aqueous solution of sodium chloride and dried on anhydrous sodium sulfate, and then the solvent was distilled off. The residue was purified by silica gel column chromatography (methylene chloride:methanol=50:1, v/v) to obtain 2-amino-9-[(1R,2R,3S)-2,3-bis(t-butyldiphenylsilyloxymethyl)-1-cyclopentyl]-6-(2-methoxyethoxy)purine (124 mg, Yield 29%).

후처리

  1. stirringthe resulting mixture was stirred at 140° C. for one hour
  2. additionwas added
  3. customthe product formed
  4. extractionwas extracted with ethyl acetate
  5. washThe extract solution was washed with water
  6. washwashed with saturated aqueous solution of sodium chloride
  7. dry with materialdried on anhydrous sodium sulfate
  8. distillationthe solvent was distilled off
  9. customThe residue was purified by silica gel column chromatography (methylene chloride

출처 및 근거

ORD 기록
ord-7312be4a5cab47549547ad4fc88cc255
출처 데이터셋
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05374625

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트