Water → HCID 22063472、化合物

HRID 1666182ノート

反応式

HRID 1666182 の反応式
C(O[CH:9]1[C:14](=[O:15])[NH:13][C:12]2[CH:16]=[CH:17][CH:18]=[C:19]([C:20](=[O:26])[CH:21](OCC)O)[C:11]=2[O:10]1)C1C=CC=CC=1.[NH2:27][C:28]([CH3:46])([CH3:45])[CH2:29][C:30]1[CH:44]=[CH:43][C:33]([O:34][CH2:35][CH2:36][CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39])=[CH:32][CH:31]=1.O.[C:48]([OH:53])(=O)[C:49](O)=O>C(OCC)(=O)C.C(OCC)C>[CH2:48]([O:53][C:17]1[CH:18]=[C:19]([CH:20]([OH:26])[CH2:21][NH:27][C:28]([CH3:45])([CH3:46])[CH2:29][C:30]2[CH:44]=[CH:43][C:33]([O:34][CH2:35][CH2:36][CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39])=[CH:32][CH:31]=2)[C:11]2[O:10][CH2:9][C:14](=[O:15])[NH:13][C:12]=2[CH:16]=1)[C:49]1[CH:18]=[CH:19][CH:11]=[CH:12][CH:16]=1

参加物

7

反応物 4

HCID 962WaterHCID 971Oxalic AcidHCID 22063453HCID 22063453、化合物HCID 22063456HCID 22063456、化合物

生成物 1

HCID 22063472HCID 22063472、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1.20 g (3.36 mmol) of benzyloxy-8-(2-ethoxy-2-hydroxyacetyl)-4H-benzo[1,4]oxazin-3-one and 0.90 g (3.22 mmol) of ethyl 4-[4-(2-amino-2-methylpropyl)phenoxy]butyrate are reacted in the manner described for Example 8(d). The crude product is dissolved in 10 mL ethyl acetate and 10 mL water and combined with oxalic acid with stirring. The solution is diluted with diethyl ether and the solid precipitated is suction filtered and washed with diethyl ether. Yield: 1.20 g (54%, oxalate); melting point 223° C.-227° C.

後処理

  1. customthe solid precipitated
  2. filtrationfiltered
  3. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-0ee7d44545bf4466aca29a61e76d63b1
出典データセット
uspto-grants-2011_10
特許番号
US08044046B2

反応ノート

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