HCID 54440772、化合物 → HCID 20077534、化合物

HRID 1655053ノート

反応式

HRID 1655053 の反応式
C[O:2][C:3]([C:5]1[CH:13]=[C:12]2[C:8]([C:9]([CH2:15][C:16]3[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]4[CH:33]=[CH:32][C:31]5[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=5)[N:25]=4)=[CH:18][CH:17]=3)=[CH:10][N:11]2[CH3:14])=[CH:7][CH:6]=1)=[O:4]>[OH-].[Na+].O1CCCC1.CO.O>[CH3:14][N:11]1[C:12]2[C:8](=[CH:7][CH:6]=[C:5]([C:3]([OH:4])=[O:2])[CH:13]=2)[C:9]([CH2:15][C:16]2[CH:17]=[CH:18][C:19]([O:22][CH2:23][C:24]3[CH:33]=[CH:32][C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[N:25]=3)=[CH:20][CH:21]=2)=[CH:10]1

参加物

6

反応物 1

HCID 54440772HCID 54440772、化合物

生成物 1

HCID 20077534HCID 20077534、化合物収率 59.7%

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of the methyl ester (Example 10, part ii) (1.73 g) in aqueous sodium hydroxide (2M, 5.9 ml), tetrahydrofuran (20 ml) and methanol (10 ml) was refluxed with stirring overnight. The reaction mixture was cooled, diluted with water until turbid and washed with diethyl ether (2×). The aqueous phase was acidified with acetic acid and the resulting precipitate filtered, washed with water and dried in vacuo at 50° C. to give the product as a white solid (1 g). A small amount was crystallised from tetrahydrofuran/ethanol m.p. 208°-212° C.

後処理

  1. temperatureThe reaction mixture was cooled
  2. washwashed with diethyl ether (2×)
  3. filtrationthe resulting precipitate filtered
  4. washwashed with water
  5. customdried in vacuo at 50° C.

出典と根拠

ORDレコード
ord-11841f544d40485eaefa555b93fd970f
出典データセット
uspto-grants-1995_04
特許番号
US05410061

反応ノート

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