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

HRID 1111683

반응식

HRID 1111683 반응식
[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

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 78597N-(Hydroxymethyl)-3,4,5,6-tetrahydrophthalimideHCID 22767648Dispiro(2.0.4.1)nonan-9-carboxylic acid

생성물 1

HCID 227676553.4,5.6-Tetrahydrophthalimidomethyl dispiro(2.0.4.1)nonane-9-Carboxylate

시약·촉매·용매 2

HCID 241Benzene용매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-aaf3ae2a005040e89a8cd44fc2b3e927
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04118510

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