Diethyl Ether → HCID 178506551、化合物

HRID 2378712ノート

反応式

HRID 2378712 の反応式
[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

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 11776TriphenylphosphineHCID 178483384HCID 178483384、化合物

生成物 1

HCID 178506551HCID 178506551、化合物収率 92.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

(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%).

後処理

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

出典と根拠

ORDレコード
ord-b24b19a4a87b4131b527251f6cf9cd43
出典データセット
uspto-grants-2008_12
特許番号
US07470717B2

反応ノート

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