Water → HCID 69619643, 화합물

HRID 585744노트

반응식

HRID 585744 반응식
[CH2:1]([O:8][C:9]([NH:11][C@@H:12]1[C:21]2[C:16](=[CH:17][C:18]([C:22]([NH:24][C:25]3[CH:30]=[CH:29][N:28]=[C:27]4[N:31](CO)[CH:32]=[CH:33][C:26]=34)=[O:23])=[CH:19][CH:20]=2)[S:15][CH2:14][CH2:13]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])(=O)C.[Na+].O>CO.O1CCCC1>[CH2:1]([O:8][C:9]([NH:11][C@@H:12]1[C:21]2[C:16](=[CH:17][C:18]([C:22]([NH:24][C:25]3[CH:30]=[CH:29][N:28]=[C:27]4[NH:31][CH:32]=[CH:33][C:26]=34)=[O:23])=[CH:19][CH:20]=2)[S:15][CH2:14][CH2:13]1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 517045Sodium AcetateHCID 20824441HCID 20824441, 화합물

생성물 1

HCID 69619643HCID 69619643, 화합물수율 70.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

The obtained (S)-4-(benzyloxycarbonylamino)-N-(1-hydroxymethylpyrrolo[2,3-b]pyridin-4-yl)thiochromane-7-carboxamide (766 mg) was dissolved in methanol (10 ml) and tetrahydrofuran (20 ml), and an aqueous solution (30 ml) of sodium acetate (5.00 g) was added. The reaction mixture was stirred under reflux for 5 hr and allowed to return to room temperature. Water (100 ml) was added and the precipitated crystals were collected by filtration to give the objective (S)-4-(benzyloxycarbonylamino)-N-(1H-pyrrolo[2,3-b]pyridin-4-yl)thiochromane-7-carboxamide (504 mg) as a pale yellow solid.

후처리

  1. temperatureunder reflux for 5 hr
  2. customto return to room temperature
  3. filtrationthe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-7d672c0d58784cd6b42033393e02f6a2
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933305B2

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