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1,2-Dichloroethane → HCID 7237625、化合物

HRID 2237372
ノート
印刷プレビュー

反応式

HRID 2237372 の反応式
C1C=CC2N(O)N=NC=2C=1.CN1CCOCC1.[CH2:18]([O:25][C:26]([NH:28][C@@H:29]([C:34]([OH:36])=O)[CH2:30][CH:31]([CH3:33])[CH3:32])=[O:27])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(Cl)CCl.Cl.[CH3:42][O:43][C:44](=[O:51])[C@H:45]([CH2:47][CH:48]([CH3:50])[CH3:49])[NH2:46]>ClCCl>[CH3:42][O:43][C:44](=[O:51])[C@H:45]([CH2:47][CH:48]([CH3:50])[CH3:49])[NH:46][C:34](=[O:36])[C@@H:29]([CH2:30][CH:31]([CH3:32])[CH3:33])[NH:28][C:26]([O:25][CH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)=[O:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 79724-Methylmorpholine2 回HCID 757711-HydroxybenzotriazoleHCID 2723695Leucine methyl ester hydrochlorideHCID 7000099N-Cbz-D-leucine

生成物 1

HCID 7237625HCID 7237625、化合物

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

HOBt (4 equivalents, 2038 mg, 15.08 mmol), N-methylmorpholine (3 equivalents, 11.3 mmol), N-benzyloxycarbonyl-D-leucine (1.0 equivalent, 1000 mg, 3.8 mmol), EDC (2 equivalents, 1441 mg, 7.5 mmol) and again N-methylmorpholine (2 equivalents, 7.5 mmol) are added successively at −10° C. to a solution of L-leucine methyl ester hydrochloride (1.1 equivalents, 753.2 mg, 4.15 mmol) in dichloromethane p.a. (20 ml). The reaction mixture warms slowly (about 12 h) to RT, whereby complete conversion of the amine component is observed by means of HPLC. The reaction mixture is concentrated, taken up in ethyl acetate (about 200 ml) and then washed with a saturated aqueous sodium hydrogen carbonate solution (once), 5% aqueous citric acid (twice), a saturated aqueous sodium hydrogen carbonate solution (once) and a saturated sodium chloride solution. The mixture is dried over sodium sulfate and filtered. The mixture is evaporated to dryness in vacuo and then dried further under high vacuum. 1483 mg (93% of theory) of the title compound are obtained, which is reacted without further purification.

後処理

  1. customThe reaction mixture warms slowly (about 12 h)
  2. customto RT
  3. concentrationThe reaction mixture is concentrated
  4. washwashed with a saturated aqueous sodium hydrogen carbonate solution (once), 5% aqueous citric acid (twice), a saturated aqueous sodium hydrogen carbonate solution (once) and a saturated sodium chloride solution
  5. dry with materialThe mixture is dried over sodium sulfate
  6. filtrationfiltered
  7. customThe mixture is evaporated to dryness in vacuo
  8. customdried further under high vacuum

出典と根拠

ORDレコード
ord-f63cd50fd4054ae9a540c0aef23a46da
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07718611B2

反応ノート

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