Water → 20-{3-[N-(4-methylhexahydrophthalimido)amino]-3-oxopropyl}-2,2,4,4-tetramethyl-7-oxa-3,20-diazadispiro[5.1.11.2]heneicosane-21-one

HRID 1707310

反応式

HRID 1707310 の反応式
[NH:1]([C:3](=[O:32])[CH2:4][CH2:5][N:6]1[C:19](=[O:20])[C:9]2([CH2:14][C:13]([CH3:16])([CH3:15])[NH:12][C:11]([CH3:18])([CH3:17])[CH2:10]2)[O:8][C:7]21[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)[NH2:2].[CH3:33][CH:34]1[CH2:44][CH2:43][CH:37]2[C:38]([O:40][C:41](=O)[CH:36]2[CH2:35]1)=[O:39].O.CCCCC>C1(C)C(C)=CC=CC=1>[CH3:33][CH:34]1[CH2:44][CH2:43][CH:37]2[C:38]([N:2]([NH:1][C:3](=[O:32])[CH2:4][CH2:5][N:6]3[C:19](=[O:20])[C:9]4([CH2:14][C:13]([CH3:15])([CH3:16])[NH:12][C:11]([CH3:18])([CH3:17])[CH2:10]4)[O:8][C:7]43[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]4)[C:41](=[O:40])[CH:36]2[CH2:35]1)=[O:39]

参加物

6

反応物 4

HCID 962Water2 回HCID 8003PentaneHCID 86876Hexahydro-4-methylphthalic anhydrideHCID 1896313820-(3-Hydrazino-3-oxopropyl)-2,2,4,4-tetramethyl-7-oxa-3,20-diazadispiro[5.1.11.2]heneicosane-21-one

生成物 1

HCID 1896314120-{3-[N-(4-methylhexahydrophthalimido)amino]-3-oxopropyl}-2,2,4,4-tetramethyl-7-oxa-3,20-diazadispiro[5.1.11.2]heneicosane-21-one

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒2 回

実験手順

The hydrazide of Example 1, 13.5 g (0.03 mole), was added to 225 ml xylene at 75° C. Added dropwise to this was 4-methylhexahydrophthalic anhydride, 5.1 g (0.03 mole) in 25 ml xylene. The apparatus was fitted with a Dean Stark water separation assembly and the reaction mixture was heated to reflux for 4 hours with azeotropic removal of water as it formed. The xylenes were stripped using aspirator vacuum and the residual sticky solid was slurried with 300 ml pentane. The solid was filtered and dried for 2 hours on the filter funnel. The white solid product weighed 11.7 g and had a melting range of 210°-212° C. The infrared spectrum (mull) showed two carbonyl bands at 1690 and 1730 cm-1.

後処理

  1. temperaturethe reaction mixture was heated
  2. customformed
  3. filtrationThe solid was filtered
  4. customdried for 2 hours on the filter funnel

出典と根拠

ORDレコード
ord-1ce6e273f96b447ca991dee7f0f7384c
出典データセット
uspto-grants-1994_10
特許番号
US05352719

関連ノート

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