1,3,3-Trimethyl-2-methyleneindoline → HCID 54308342、化合物

HRID 355604

反応式

HRID 355604 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH3:12])([CH3:11])[C:3]1=[CH2:13].[OH:14][C:15]1[CH:27]=[C:26]([N:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)[C:18]2[O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[C:17]=2[C:16]=1[N:34]=O>CO>[CH3:1][N:2]1[C:3]2([CH2:13][NH:34][C:16]3[C:17]4[C:21]5[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=5[O:19][C:18]=4[C:26]([N:28]4[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]4)=[CH:27][C:15]=3[O:14]2)[C:4]([CH3:11])([CH3:12])[C:5]2[C:10]1=[CH:9][CH:8]=[CH:7][CH:6]=2

参加物

4

反応物 2

HCID 83511,3,3-Trimethyl-2-methyleneindolineHCID 18940154HCID 18940154、化合物

生成物 1

HCID 54308342HCID 54308342、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 1,3,3-trimethyl-2-methyleneindoline (0.435 g; 0.0025 mol) and 2-hydroxy-1-nitroso-4-piperidinodibenzofuran (0.675 g; 0.0025 mol) in methanol (25.0 ml) was heated under nitrogen and refluxed with stirring for 41 hours. The solution was evaporated to dryness and chromatographed over silica (eluent: dichloromethane) to yield 1,3,3-trimethyl-6'-piperidinospiro[2H-indole 2,3'-[3H]-[2H-[1,4]benzoxazino [6,5-b]benzofuran]] as an amber oil (0.35 g; 32%), which afforded a pale yellow solid upon trituration with diethyl ether, m.pt. 213.5°-216° C.; λmaxAbsorbance 570 nm (Polyurethane). ##STR13##

後処理

  1. temperaturewas heated under nitrogen
  2. temperaturerefluxed
  3. customThe solution was evaporated to dryness
  4. customchromatographed over silica (eluent: dichloromethane)

出典と根拠

ORDレコード
ord-6d92b1e8128649b898aed0a45b3cb96d
出典データセット
uspto-grants-1998_11
特許番号
US05833885

関連ノート

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