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Sodium Acetate → 4-N-(Carbomethoxymethyl)-6-(carboethoxy-3-phenylpropylamino)-perhydro-1,4-thiazepin-5-one

HRID 1981891
ノート
印刷プレビュー

反応式

HRID 1981891 の反応式
FC(F)(F)[C:3]([OH:5])=[O:4].[NH2:8][CH:9]1[CH2:15][S:14][CH2:13][CH2:12][N:11]([CH2:16][C:17]([O:19][CH3:20])=[O:18])[C:10]1=[O:21].[C:22]([O-])(=O)[CH3:23].[Na+].O=[C:28]([CH2:34][CH2:35][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)C(OCC)=O.C([BH3-])#N.[Na+]>CO>[C:17]([CH2:16][N:11]1[C:10](=[O:21])[CH:9]([N:8]([C:3]([O:5][CH2:22][CH3:23])=[O:4])[CH2:28][CH2:34][CH2:35][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH2:15][S:14][CH2:13][CH2:12]1)([O:19][CH3:20])=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 517045Sodium AcetateHCID 562087Ethyl alpha-oxobenzenebutanoateHCID 5003444Sodium cyanoborohydrideHCID 136337346-Amino-4-N-(carbomethoxymethyl)-perhydro-1,4-thiazepin-5-one, Trifluoroacetate Salt

生成物 1

HCID 233180554-N-(Carbomethoxymethyl)-6-(carboethoxy-3-phenylpropylamino)-perhydro-1,4-thiazepin-5-one

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒
2 回

実験手順

6-Amino-4-N-(carbomethoxymethyl)perhydro-1,4-thiazepin-5-one, trifluoroacetate salt (0.166 g), sodium acetate (0.04 g), and ethyl 2-keto-4-phenylbutyrate are dissolved in 1 ml of methanol. After 1/2 hour at room temperature, a solution of sodium cyanoborohydride (0.16 g) in 0.5 ml of methanol is added dropwise over a period of one hour. At the end of seven hours, the reaction mixture is partitioned between chloroform and water. The aqueous phase is adjusted to pH 10 with sodium bicarbonate. The organic layer is separated and washed two more times with water. After chromatography on silica gel (1:1 ethyl acetate-hexanes), the product is obtained as an oil (0.17 g). The NMR spectrum shows a singlet at 7.2, complex absorption between 3.7 and 4.4, a multiplet between 3.1 and 3.4, a multiplet between 3.6 and 3.9, a multipet between 1.9 and 2.2, and a triplet at 1.3.

後処理

  1. customAt the end of seven hours, the reaction mixture is partitioned between chloroform and water
  2. customThe organic layer is separated
  3. washwashed two more times with water

出典と根拠

ORDレコード
ord-96d442a62f96407f978cde1beddc0b11
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04594341

反応ノート

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