1,2-Dichloroethane → HCID 58333428、化合物

HRID 2066850ノート

反応式

HRID 2066850 の反応式
[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28](O)=[O:29])=[CH:23][C:22]=3[F:31])[CH2:17][CH2:16]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2].[CH3:32]OC(=O)CN.C1C=C[C:41]2[N:46](O)N=[N:44][C:42]=2C=1.C(Cl)CCl>C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:8][CH2:9][CH:10]([O:13][N:14]=[C:15]2[CH2:16][CH2:17][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28](=[O:29])[NH:46][CH2:41][CH2:42][NH:44][CH3:32])=[CH:23][C:22]=3[F:31])[CH2:19][CH2:20]2)[CH2:11][CH2:12]1)=[O:6])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 69221Glycine methyl esterHCID 757711-HydroxybenzotriazoleHCID 58333593HCID 58333593、化合物

生成物 1

HCID 58333428HCID 58333428、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

9-1 (32 mg, 0.073 mmol), amino-acetic acid methyl ester (0.11 mmol) and HOBT (15 mg, 0.11 mmol) were combined in DCM (1 mL) and stirred at room temperature for 10 minutes. EDC(19 mg, 0.1 mmol) was added and the mixture was stirred for 18 h. The solution was washed with 2 mL of aqueous NaHCO3, concentrated and taken up with 1 mL of DCM. 1 mL of TFA was added and the mixture was stirred at room temperature for 1 h. It was then concentrated under a stream of nitrogen and purified on preparative HPLC to give 31-1: LC-MS 496.5 (MH).

後処理

  1. stirringthe mixture was stirred for 18 h
  2. washThe solution was washed with 2 mL of aqueous NaHCO3
  3. concentrationconcentrated
  4. addition1 mL of TFA was added
  5. stirringthe mixture was stirred at room temperature for 1 h
  6. concentrationIt was then concentrated under a stream of nitrogen
  7. custompurified on preparative HPLC
  8. customto give 31-1

出典と根拠

ORDレコード
ord-aad03f2391444b89879c616189bea6c2
出典データセット
uspto-grants-2012_10
特許番号
US08293729B2

反応ノート

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