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

HRID 1603878노트

반응식

HRID 1603878 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-84f6047b08b24789b0df33ef750b002f
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990142

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