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Sodium Hydroxide → 2-Diphenylphosphinylmethyl-2'-methyl-1,1'-binaphthyl

HRID 2397
ノート
印刷プレビュー

反応式

HRID 2397 の反応式
[Br-].[C:2]1([P+:8]2([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH2:14][C:13]3[CH:15]=[CH:16][C:17]4[C:22]([C:12]=3[C:11]3[C:23]5[CH:24]=[CH:25][CH:26]=[CH:27][C:28]=5[CH:29]=[CH:30][C:10]=3[CH2:9]2)=[CH:21][CH:20]=[CH:19][CH:18]=4)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-:37].[Na+]>C(O)C>[C:2]1([P:8]([CH2:9][C:10]2[CH:30]=[CH:29][C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[C:11]=2[C:12]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH:16]=[CH:15][C:13]=2[CH3:14])([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[O:37])[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 110060894,4-diphenyl-4,5-dihydro-3H-dinaphtho-[2,1-c:1',2'-e]phosphepinium bromide

生成物 1

HCID 157892202-Diphenylphosphinylmethyl-2'-methyl-1,1'-binaphthyl

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4 g (7.3 mmol) of 4,4-diphenyl-4,5-dihydro-3H-dinaphtho-[2,1-c:1',2'-e]phosphepinium bromide are suspended in a mixture of 80 ml of 2N sodium hydroxide solution and 30 ml of ethanol and heated to boiling for 4 hours. The reaction solution is subsequently evaporated to dryness at 12 torr/40° C. The residue is taken up in 80 ml of dichloromethane and extracted twice with 30 ml of water each time. The organic phase is dried over sodium sulfate and evaporated to dryness at 12 torr/40° C. This gives colorless crystals (melting point: 199.5° C.).

後処理

  1. temperatureheated
  2. customThe reaction solution is subsequently evaporated to dryness at 12 torr/40° C
  3. extractionextracted twice with 30 ml of water each time
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customevaporated to dryness at 12 torr/40° C

出典と根拠

ORDレコード
ord-86e31c9534414a65b91ab486505f6497
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05728886

反応ノート

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