Sodium Hydroxide → 8-[2-(Benzyloxymethyl)chromane-6-carboxamido]-4-oxo-4H-1-benzopyran-2-carboxylic acid

HRID 1603878ノート

反応式

HRID 1603878 の反応式
[CH2:1]([O:8][CH2:9][CH:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:20]([NH:22][C:23]3[C:32]4[O:31][C:30]([C:33]([O:35]CC)=[O:34])=[CH:29][C:28](=[O:38])[C:27]=4[CH:26]=[CH:25][CH:24]=3)=[O:21])[CH:16]=2)[O:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CO.O1CCCC1>[CH2:1]([O:8][CH2:9][CH:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:20]([NH:22][C:23]3[C:32]4[O:31][C:30]([C:33]([OH:35])=[O:34])=[CH:29][C:28](=[O:38])[C:27]=4[CH:26]=[CH:25][CH:24]=3)=[O:21])[CH:16]=2)[O:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 19606281Ethyl 8-[2-(benzyloxymethyl)chromane-6-carboxamido]-4-oxo-4H-1-benzopyran-2-carboxylate

生成物 1

HCID 196063368-[2-(Benzyloxymethyl)chromane-6-carboxamido]-4-oxo-4H-1-benzopyran-2-carboxylic acid収率 97%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of ethyl 8-[2-(benzyloxymethyl)chromane-6-carboxamido]-4-oxo-4H-1-benzopyran-2-carboxylate (0.240 g, 0.47 mmol) in a mixture of methanol (15 ml) and tetrahydrofuran (15 ml) was added with 0.510 ml of a 1M NaOH solution, stirring at room temperature for 1.30 h. After that the mixture was evaporated to dryness and the resulting residue was suspended in water adding 0.2M hydrochloric acid to slightly acid pH (pH=4-5). The solid was recovered by filtration, washed with methanol and dried on phosphorous pentoxyde under vacuum, thereby obtaining 0.221 g of the title compound as a white solid which decomposes above 283° C. (97% yield).

後処理

  1. customAfter that the mixture was evaporated to dryness
  2. filtrationThe solid was recovered by filtration
  3. washwashed with methanol
  4. customdried on phosphorous pentoxyde under vacuum

出典と根拠

ORDレコード
ord-84f6047b08b24789b0df33ef750b002f
出典データセット
uspto-grants-1999_11
特許番号
US05990142

反応ノート

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