Water → HCID 69619643、化合物

HRID 585744ノート

反応式

HRID 585744 の反応式
[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

参加物

6

反応物 3

HCID 962WaterHCID 517045Sodium AcetateHCID 20824441HCID 20824441、化合物

生成物 1

HCID 69619643HCID 69619643、化合物収率 70.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-7d672c0d58784cd6b42033393e02f6a2
出典データセット
uspto-grants-2005_08
特許番号
US06933305B2

反応ノート

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