Diethyl Ether → HCID 178506551, 화합물

HRID 2075429노트

반응식

HRID 2075429 반응식
[I-:1].[NH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH2:11][N+](C)(C)C)=[N:3]1.[C:16]1([P:22]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(OCC)C>CN(C=O)C>[I-:1].[NH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH2:11][P+:22]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)=[N:3]1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 11776TriphenylphosphineHCID 178483384HCID 178483384, 화합물

생성물 1

HCID 178506551HCID 178506551, 화합물수율 92.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

(1H-indazol-3-ylmethyl)trimethylammonium iodide (45.0 g, 142 mmol) obtained in Step 3 was dissolved in DMF (220 mL), and the solution was mixed with triphenylphosphine (44.7 g, 170 mmol), followed by heating under reflux for 2.5 hours. After cooling to room temperature, the reaction mixture was added with diethyl ether and was stirred overnight. The resulting precipitates were collected by filtration to obtain (1H-indazol-3-ylmethyl)triphenylphosphonium iodide (68.3 g, 92%).

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 2.5 hours
  3. customThe resulting precipitates
  4. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-6cf140caf25b4122879656a4d6123778
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07919517B2

반응 노트

불러오는 중…