Triethylamine → 3.4,5.6-Tetrahydrophthalimidomethyl dispiro(2.0.4.1)nonane-9-Carboxylate

HRID 1111683

反応式

HRID 1111683 の反応式
[CH2:1]1[C:3]2([CH:9]([C:10]([OH:12])=[O:11])[C:4]32[CH2:8][CH2:7][CH2:6][CH2:5]3)[CH2:2]1.S(Cl)(Cl)=O.O[CH2:18][N:19]1[C:23](=[O:24])[C:22]2[CH2:25][CH2:26][CH2:27][CH2:28][C:21]=2[C:20]1=[O:29].C(N(CC)CC)C>C1C=CC=CC=1.CCOCC>[CH2:2]1[C:3]2([CH:9]([C:10]([O:12][CH2:18][N:19]3[C:20](=[O:29])[C:21]4[CH2:28][CH2:27][CH2:26][CH2:25][C:22]=4[C:23]3=[O:24])=[O:11])[C:4]32[CH2:5][CH2:6][CH2:7][CH2:8]3)[CH2:1]1

参加物

7

実験手順

Dispiro(2.0.4.1)nonan-9-carboxylic acid (0.66g) was converted to the corresponding acid chloride by refluxing with thionyl chloride (1ml) in benzene (20 ml) for 1 hour. The acid chloride, N-hydroxymethyl-3,4,5,6-tetrahydrophthalimide (0.7g) and triethylamine (0.5g) were then stirred together in ether (50 ml) for 6 hours. After removal of solvent under reduced pressure the residue was purified by chromatography on silica gel using dichloromethane as eluent. The required product was obtained as an oil R.I. nD18 1.5318.

後処理

  1. customAfter removal of solvent under reduced pressure the residue
  2. customwas purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-aaf3ae2a005040e89a8cd44fc2b3e927
出典データセット
uspto-grants-1978_10
特許番号
US04118510

関連ノート

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