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Acetic Acid → 4-(6-Hexanamido-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)-3-hydroxybenzoic acid

HRID 1646366
ノート
印刷プレビュー

反応式

HRID 1646366 の反応式
C([Li:5])CCC.[CH2:6]([SH:8])[CH3:7].[C:9]([NH:16][C:17]1[CH:18]=[CH:19][C:20]2[O:25][CH2:24][CH2:23][N:22]([CH2:26][C:27]3[CH:36]=[CH:35][C:30]([C:31]([O:33]C)=[O:32])=[CH:29][C:28]=3[O:37]C)[C:21]=2[CH:39]=1)(=[O:15])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].C(O)(=O)C>CN1C(=O)N(C)CCC1.O>[S-:8][CH2:6][CH3:7].[Li+:5].[C:9]([NH:16][C:17]1[CH:18]=[CH:19][C:20]2[O:25][CH2:24][CH2:23][N:22]([CH2:26][C:27]3[CH:36]=[CH:35][C:30]([C:31]([OH:33])=[O:32])=[CH:29][C:28]=3[OH:37])[C:21]=2[CH:39]=1)(=[O:15])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 176Acetic AcidHCID 6343EthanethiolHCID 23365905Methyl 4-(6-hexanamido-2,3-dihydrobenz-1,4-oxazin-4ylmethyl)-3-methoxybenzoateHCID 178418339Butyllithium

生成物 2

HCID 10866251Lithium thioethoxideHCID 233658934-(6-Hexanamido-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)-3-hydroxybenzoic acid
収率 36%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-溶媒2 回

実験手順

Lithium thioethoxide was prepared by the dropwise addition of n-butyllithium (4 ml. of 1.53 molar solution in hexane) to a stirred solution of ethyl mercaptan (0.5 ml.) in dry N,N'-dimethylpropylene urea (DMPU) (9 ml.), under a nitrogen atmosphere. A solution of methyl 4-(6-hexanamido-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)-3-methoxybenzoate (prepared as described in Example 26) (0.35 g.) in DMPU (3 ml.) was added, the mixture stirred at ambient temperature for 15 minutes, then heated to, and maintained at, 130° C. for 4 hours. The cooled mixture was diluted with water, acidified with acetic acid, extracted with ethyl acetate, the extracts washed with water, dried (MgSO4) and evaporated. The product was purified by flash chromatography on silica gel, eluting with 80:20:2 v/v/v toluene:ethyl acetate:acetic acid, giving a white solid which was washed with hexane and dried, to give the title compound (0.114 g., 36%) as a white solid, m.p. 183°-184° C.

後処理

  1. temperatureheated to, and
  2. temperaturemaintained at, 130° C. for 4 hours
  3. extractionextracted with ethyl acetate
  4. washthe extracts washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe product was purified by flash chromatography on silica gel
  8. washeluting with 80:20:2 v/v/v toluene
  9. customethyl acetate:acetic acid, giving a white solid which
  10. washwas washed with hexane
  11. customdried

出典と根拠

ORDレコード
ord-258c389889d54c909ce2379fa7b49020
出典データセット
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05179112

反応ノート

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